00
m<OU 168448 m
Copyright, 1935, by
D. VAN NOSTRAND COMPANY, INC.
All Rights Reserved
This book, or any part thereof, may
not be reproduced in any form without
written permission from the publishers.
Printed in TJ. S. A.
PREFACE
It is hoped that the present volume will, in a sense, serve to
mark the end of an era, and the beginning of a new one. Man-
kind has had certain arts from time immemorial. Weaving,
smelting, pottery, and the production of alcoholic beverages are
noteworthy among these. And they share, besides great age,
the distinction of having reached a fairly high peak of perfection
without that intensive application of scientific development which
has been characteristic of the newer arts whose origin has been
in the advance of scientific knowledge.
This is not to say that they have been untouched by science
until the twentieth century. In particular the art of alcoholic
beverages owes much to the workers of the nineteenth century.
Pasteur, Hansen, Lavoisier, and many of the immortals of sci-
ence have left their imprint and monuments in this field as well
as in many others. More recently, but still apart from the mod-
ern age were the great investigations by the Royal Commission
in Great Britain and President Taft's Board in this country into
the question "What is Whiskey?" In our wine production, the
work of the beloved Harvey W. Wiley culminating in the "Amer-
ican Wines at the Paris Exposition" had a far-reaching decisive
effect. This summary cannot do more than pay its respects to
the thousands of earnest workers here and abroad who by their
labors have added vastly to our knowledge of the art of making
alcoholic beverages and their composition.
The beverage art, however, has been distinguished in an-
other way. It has had to suffer under the inherent conservative
tendency of any old art, and also it has been specially hampered
by various legal bedevilments. The era just past in the United
States, prohibition, may be likened, by not a too strained analogy,
to the Dark Ages in Europe from the fourth to the fourteenth
IV
PREFACE
century. During the prohibition period, the beverage art, under
the necessity of continuing its existence to satisfy a demand
which would not cease even at an official behest, and yet under
the need of concealment to evade legal requirements, went
through a curious semi-comatose state.
The time happened to coincide with a period in our national
life when in all other arts, the sciences, especially the science of
chemistry and the growing knowledge of chemical engineering,
were finding broad new fields of extensive and intensive applica-
tion. The vast results of these applications both in new products
and in increased and improved productiveness are too well known
to require illustration.
Hence the repeal of prohibition found the beverage art as a
sort of stepchild. Chemical science was ready to step in. Chem-
ical engineering had its techniques ready. But the art to which
these were to be applied was demoralized. Bootlegging required
very little of its product. A very bare resemblance to its proto-
type and a substantial "kick" were sufficient to satisfy the market.
Quality of product was generally unattainable by bootleg manu-
facturer, and really unnecessary to his market. Economy of
production was a relatively minor consideration when the liability
to government seizure and the maintenance of an army of thugs
and wholesale bribery constituted the larger items in the final
selling price of the product.
In this historical background, the present volume is offered.
The authors are unaware of any other summary of the art as it
now exists which has been published recently and they feel that
there may be a need for it. On this account the authors have
felt it necessary to include between the same covers a wide di-
versity of material of varying degrees of technical density, and
they have been thereby forced to an equal diversity of treatment.
Those sections which are primarily descriptive are necessarily
broad rather than detailed. On the other hand, in the analytical
sections, for example, precision of detail has been a specific aim.
With this rationale for its apparent lack of uniformity, the au-
thors offer it to the scientists and engineers who may within the
next few decades largely transform the beverage art, in the hope
OSMANIA UNIVERSITY LIBRARY
Call No. && &/ if I & Accession No
I t - ^ -A /-
Author
Title
* This book should be returned on or before the date last marked below.
CHEMISTRY AND TECHNOLOGY
OF WINES AND LIQUORS
PREFACE
V
that for them it will prove a useful starting point. To the larger
number who may wish to have a general knowledge of existing
techniques or to have handy a reference for special purposes, the
volume is also introduced in the hope that they will find in it such
information as they may need.
February, 1935.
CONTENTS
CHAPTER PAGE
PREFACE iii
LIST OF TABLES ix
LIST OF FIGURES . xi
I. THEORETICAL CONSIDERATIONS. SUGARS AND STARCHES . 3
II. THEORETICAL CONSIDERATIONS. ENZYMES . . . 13
III. THEORETICAL CONSIDERATIONS. FERMENTATION . . 17
IV. THEORETICAL CONSIDERATIONS. RAW MATERIALS . . 25
V. YEASTS AND OTHER ORGANISMS 46
VI. PRODUCTION OF YEAST 63
VII. MALT 71
VIII. DISTILLATION 79
IX. WHISKEY MANUFACTURE 96
X. BRANDY, RUM, GIN, APPLEJACK AND MINOR DISTILLED
LIQUORS 139
XI. WINES, CHAMPAGNE AND CIDER 155
XII. LIQUEURS AND CORDIALS 190
XIII. ANALYSIS OF ALCOHOLIC BEVERAGES. INTERPRETATION . 230
XIV. ANALYSIS OF ALCOHOLIC BEVERAGES. METHODS . . 260
ANALYTICAL REFERENCE TABLES 298
XV. STATISTICS OF THE LIQUOR INDUSTRY 326
SELECTED BIBLIOGRAPHIES 34-8
INDEX 355
vii
TABLES
TABLE PAG i
I. Composition of Barley 28
II. Composition of Rye 30
III. Composition of Corn 32
IV. Composition of Oats 33
V. Composition of Wheat 35
VI. Comparative Table of Cereal Compositions . . 36
VII. American Grape Varieties 38
VIII. Comparison of Whiskey Processes 102
IX. Composition of Wine Musts 162
X. Analyses of Whiskies (Schidrowitz) .... 242-6
XL Maxima and Minima on Scotch Whiskies . . . 247
XII. Analyses of Whiskies (Tatlock 248
XIIL Average, Maxima and Minima Data on Rye Whiskies
(Crampton and Tolman) 250
XIV. Average, Maxima and Minima Data on Bourbon
Whiskies (Crampton and Tolman) . . . .251
XV. Analysis of Eaux-de-vie De Vin of Known Origin . . 252
XVI. Analysis of Eaux-de-vie of Known Origin . . . 253
XVII. Analysis of Components of 25 Year Old Brandy . . 254
XVIII. Analyses of Jamaica Rum 254
XIX. Analyses of Demerara Rum 255
XX. Analyses of Martinique Rum 255
XXL Compiled Data on Rum ....... 256
XXII. Analysis of Gin 256
XXIII. Average Composition of European Wines . . .257
XXIV. Average Composition of California Wines . . . 258
XXV. Analyses of Liqueurs 259
XXVI. Average Composition of Liquers 259
Ai. Refractometer Readings of Methyl-Ethyl Alcohol
Mixtures 294
A2. Densities of Sugar Solutions 298-301
A3. Specific Gravities of Alcohol-Water Mixtures at
15-56/15.56 c 302-3
A4. Specific Gravities of Alcohol-Water Mixtures at
20/20 C. 304-5
ix
x TABLES
TABLE PAGE
A5. Specific Gravities of Alcohol-Water Mixtures at
25/25 C 306-7
A6. Refractometer Readings of Alcohol-Water Mixtures at
Several Temperatures 308-19
A;. Munson and Walker's Table .... 320-25
XXVII. Distilleries and Industrial Alcohol Plants in U. S.
1901-32 331
XXVIII. Taxes Paid on Wines and Liquors in U. S. 1901-1932 332
XXIX. Spirits in Bond in U. S. 1901-1932 .... 333
XXX. Materials Consumed in Alcohol Manufacture in U. S.
1901-1932 334-5
XXXI. Distilled Spirits Produced in U. S. 1901-1932 . . 336
XXXII. Withdrawals of Tax Paid Spirits. 1901-1932 . . 337
XXXIII. Exports of Distilled Spirits. 1901-1932 .... 338
XXXIV. Whiskey Exports by Country of Destination. 1904-
1932 339-41
XXXV. Imports of Liquors. 1901-1932 342
XXXVI. Apparent U. S. Consumption of Distilled Spirits. 1901-
1932 343
XXXVII. Wine Statistics. 1912-1932 344
XXXVIII. Wine Exports. 1901-1925 345
XXXIX. Wine Imports. 1901-1931 346
XL. Apparent U. S. Wine Consumption. 1912-1932 . . 347
XLI. International Trade in Wine. 1930 .... 347
TEXT FIGURES
FIGURE PAC7E
1. Hydrolytfc Products of Starch n
2. Wine Yeasts 49
3. Harmful Organisms 54
4. Grape Molds 58
5. Bacteria of Wine Diseases 59
6. Flow Sheet of Yeast Manufacture ...... 64
T. Flow Sheet of Distillers' Yeast Manufacture .... 66
8. Cross Section of Barley Kernel 72
9. Changes During Malting 73
10. Flow Sheet of Malting Process 75
lOa. Water Alcohol Boiling Point Curve 80
lob. Alcohol Content of Vapor from Boiling Dilute Alcohol
Solutions 8 1
n. Simple Pot Still 82
12. Pot Still with Chautfe-Vin 83
13. Pot Still with Chauffe-Vin 84
14. Pot Still as used for Scotch Whiskey 85
15. Pot Still with retorts, rectifiers and condensers .... 86
16. Pot Still with double retort 86
1 7. Pot Still with Corty's Head 86
18. Coffey's Patent Still 88
19. Diagram of Coffey's Still 89
20. Beer Still 91
21. Modern Intermittent Still 92
22. Continuous Ethyl Alcohol Still 94
22a. Mash Tun 102
23. Flow Sheet of Mashing at An All Malt Pot Still Distillery . 104
24. Flow Sheet for Three Types of Pot Still Whiskey . 108
25. Mashing by the Acid-Conversion Process in
26. Diagram Plan of Large Scale Distillery 118
27. Detail of Grain Storage and Milling . . . . . .118
28. Detail of Mashing, Yeasting and Fermenting . . . .119
29. Detail of Distillation for Whiskey I2O
30. Detail of Spirit and Gin Distillation 12 1
xii TEXT FIGURES
FIGURE PAGE
31. Barreling and Bottling 122
32. Detail of Mash Slop Recovery 123
33. Cyclic Mashing 125
34. Diagram of Gin Still Unit 151
35. Applejack Still 163
353. Chemical Changes from Grape Juice to Wine .... 164
36. Flow Sheet of Red Wine Manufacture 165
37. Large Modern Fermenting Room 167
38. Modern Wine Storage Room 171
39. Flow Sheet of White Wine Manufacture 173
40. Flow Sheet of Champagne Manufacture 180
41. The Vintage in the Champagne 182
42. The Tuage or Bottling of Champagne 184
43. Turning Champagne Bottles . .185
44. Disgorging and Finishing Champagne 186
45. Liqueur Blending Vessel (Conge a trancher) . . . .195
46. Cone Filter for Liqueurs 199
47. Wire Mesh Filter for Liqueurs 199
48. Filter of Fig. 47 in Use 199
49. Modern Distillery Laboratory 231
50. Apparatus for Determination of Volatile Acids .... 280
CHAPTER I
THEORETICAL CONSIDERATIONS. SUGARS AND
STARCH
General Statement. The entire wine and liquor industry
rests on the fact of nature that under suitable conditions sugar is
transformed into potable alcohol, while at the same time the
other materials in the sugar solution and the by-products result-
ing along with the alcohol lend various pleasant characteristics to
the finished product. It follows, then, that the character of the
finished product depends, first, on the raw material which fur-
nishes the sugar, second, on the conditions of the transformation
of the sugar into alcohol, and third, on the after treatment of
the alcoholic solution. An exact knowledge of the effect of each
of these factors is the key to the successful production of a uni-
formly palatable result.
Fermentation. Basically, the transformation of sugar into
alcohol is the one step which is common to all liquor production.
This change, which is only one of a vast number of similar
changes resulting from the action of living bodies on suitable
organic (carbon, hydrogen and oxygen) compounds, is called alco-
holic fermentation to distinguish it from the many similar proc-
esses which, starting with different chemicals, result in different
products.
Sugars. Alcoholic fermentation involves the transformation
of a sugar, usually dextrose, into alcohol. Hence some discussion
of sugars is the logical starting point. We have used the term
sugar in a more generalized sense than it is used in lay language.
To the chemist there are known many sugars, all of which are
chemical compounds containing carbon, hydrogen and oxygen.
The two latter elements are present always in the same ratio as
in water, so that the sugars corne into a broad classification of
3
4 SUGARS AND STARCH
chemical compounds called carbohydrates. Within this larger
group the sugars are generally distinguished by their ability to
form crystals. The chemist classifies sugars, first, according to
the number of carbon atoms contained in their molecules, and
second, according to the number of carbon atom chains which are
present in their molecule. This system of classification leads to
the following schematic terminology:
Monosaccharides
Trioses C 3 H 6 O 3 Glycerose
Tet roses C 4 H 8 O 4 Erythrose, etc.
Pentoses C 5 H 10 O 5 Arabinose, Xylose, Rhamnose, etc.
Hexoses C 6 H 12 O 6 Dextrose, Fructose, Mannose, Galactose,
etc.
Heptoses C 7 H J4 O7 Manno-heptose, Gluco-heptose, etc.
Octoses C 8 H 16 O 8 Gluco-octose, etc.
Disaccharides
Hexabioses C 12 H 2 2O ll Sucrose, Maltose, Lactose, etc.
Trisaccharides
Hexatrioses C 18 H 32 O 16 Raffinose, Melezitose, etc.
Poly-saccharides
(C 6 H 12 O 6 ) n Starch, Inulin, Cellulose, etc.
Within each group the sugars are distinguished from each
other by differences in chemical structure which result in differ-
ences of such properties as solubility, sweetness, crystal form,
optical rotating power, melting point, etc. In particular, it has been
found that for each structure there are pairs of sugars which have
equal but opposite optical rotating powers. Usually only one of
each pair is of common occurrence. Further discussion of the
chemistry of the sugars is beside our point here, which considers
them merely as raw materials for the production of alcohol.
For this purpose only the hexoses are directly suitable. Such
di- or poly-saccharides as can be converted readily into hexoses
are, of course, also of primary importance. The common hexoses
SUGARS 5
which are often encountered in the fermentation industry are, in
order of decreasing importance:
Dextrose
d-Fructose, Laevulose
Galactose.
Of the disaccharides :
Maltose
Sucrose (Saccharose)
Lactose, are of importance.
Starch is the chief poly-saccharide encountered in the fermen-
tation industry.
Hexoses. Dextrose occurs naturally in the juice of fruits
(grapes, etc.), from which is derived its common name, grape
sugar; and in blood and many other sources. It is prepared com-
mercially by the hydrolysis of starch by means of dilute acid and
can be bought in crystal form of very nearly the same high degree
of purity as cane sugar (sucrose). Its sweetness is slightly less
than that of cane sugar. More often, however, dextrose is pre-
pared directly in the wort (fermentation liquor) and converted
into alcohol without isolation. In pure solution dextrose may be
determined from the specific gravity or refractive index of the
solution. In ordinary solutions dextrose may be separately deter-
mined by making use of its chemical reducing power, optical rota-
tion, fermentability, etc. Ordinarily the fermentation industry
is more interested in the total content of fermentable sugars
than in any special one.
d-Fructose is usually also present in fruit juices, makes up
very nearly half the sweetness of honey and is obtained in equal
amounts as dextrose by the hydrolysis (so-called inversion) of
cane sugar. It is somewhat sweeter to the taste than cane sugar.
With dextrose, to which it is structurally, a very close relative, it
is the most readily fermentable of sugars.
Galactose. This sugar occurs almost exclusively as a product
of the hydrolysis of lactose, milk sugar. It is of rather minor
importance except in the production of such beverages as koumiss,
etc. by the fermentation of milk.
6 SUGARS AND STARCH
Hexabioses. Maltose. Almost the sole occurrence of this
sugar is in the product of the hydrolysis of starch either by the
action of enzymes or by acid hydrolysis. It is not isolated but is
fermented in the solution in which it is prepared. The enzyme,
maltase, is usually elaborated by the same yeasts as carry on the
fermentation. This enzyme converts the maltose into two equiva-
lents of dextrose which are then directly fermentable. When
isolated, maltose forms hard white crystalline masses, very simi-
lar to grape sugar. It is determinable by the facts that its
solutions have some reducing power (about two-thirds that of
glucose), and that its solutions are strongly dextro-rotary.
Sucrose (Saccharose). This is the sugar which is commonly
meant when the word sugar is used. It occurs naturally in sugar-
cane, beets, sugar maple, sorghum and in many other plants. Its
production and purification are among the world's major indus-
tries. Cane-sugar crystallizes in large monoclinic prisms which
are readily soluble in water, very sweet in taste, and, as marketed,
represents probably the nearest approach to absolute purity of
all materials sold in large bulk. It is determinable in pure solu-
tion by either the specific gravity, polarization, or refractive index
of its solution. In impure solution, its optical rotatory power,
lack of reducing property and the change in both these properties
after hydrolysis (inversion) furnish means of determination.
The inversion of sucrose results either from the action of
acid or of a special enzyme, invertase, which is present in yeast.
In either case the process results in one equivalent each of dex-
trose and fructose. Sucrose, itself, does not ferment, that is,
does not break up into alcohol and carbon dioxide under the
influence of the enzyme, zymase. However, since most yeasts
also contain invertase, the fermentation of sucrose proceeds as
soon as this latter enzyme has had a little time to act.
Lactose. Milk-sugar or lactose is found naturally, as its
name indicates, in milk. It forms small white crystals which dis-
solve with some difficulty in water. Lactose, on hydrolysis,
yields equivalent amounts of dextrose and galactose. After
hydrolysis the dextrose and galactose can be fermented with the
production of alcohol, and usually in practice, with some pro-
STARCH 7
duction also of lactic acid. To this change is due the special
character of beverages like koumiss.
Starch.-; While many fermented liquors obtain sugar for con-
version into alcohol from sources indicated above; by far the
largest single source of sugar, especially for distilled liquors, is
the poly-saccharide, starch. Its importance arises from the fact
that by suitable treatment almost 100% conversion of starch
into fermentable sugars, dextrose, maltose, etc. can be obtained.
Hence the general nature, occurrence and physical and chemical
properties of starch are of major interest in the fermented liquor
industry.
General Statement. Starch is the compound in which all of
the higher (green-leaved) plants store the sugar they need for
food. Hence it occurs almost universally in their tissues; and
in their special storage places, seeds and tubers, makes up the
bulk of the solids. When pure, it is a fine white powder having
a density of 1.6 and at ordinary temperature it is quite insoluble
in water, alcohol, ether, and other common solvents. Under the
microscope, starch appears as minute, white, translucent grains
varying widely in size and shape according to its origin. In
each case, however, the average size and shape of the starch
grains is so characteristic that it is usually comparatively easy
to determine their botanic origin. Morphologically, starch
granules can be classified into the following groups :
(1) The potato group large oval granules, showing concentric rings
and a nucleus or hilum, eccentrically placed. This group includes the
arrowroot and potato starches.
(2) The legume group round or oval granules usually also showing
concentric rings and with an irregular hilum. The starches of peas, beans
and lentils belong in this group.
(3) The wheat group round or oval granules with a central hilum.
Wheat, barley, rye and acorn as well as the starches of many medicinal
plants are found in this group.
(4) The sago group round or oval granules truncated at one end.
The group includes sago, tapioca and cinnamon starches.
(5) The rice group small, angular, polygonal grains. Corn, rice,
buckwheat and pepper starches are included in this group.
8 SUGARS AND STARCH
Within various groups the grain size may vary from 0.005-
0.15 mm. or more.
Structure. The structure of the granules is quite complex,
but consists essentially of an envelope of rather condensed nature
enclosing a colloidal substance of slightly more diffuse structure.
The envelope constitutes approximately 2% of the substance of
the granule.
Properties. The outstanding physical property of starch is
that of forming a paste when heated in the presence of water.
It can be shown under the microscope, that what happens is that
the granulose, the interior material of the granule, swells as it
absorbs water, and finally bursts its shell. A similar result can
be obtained without the use of heat if the starch is first ground
in a ball mill to break the cell wall, or if it is treated with chemi-
cal reagents which destroy the cell wall. Dilute caustic alkalies
and solutions of zinc chloride are among the reagents which
produce this result.
The temperature range required to produce pastification and
the viscosity of the resulting paste are highly characteristic of
the variety of starch employed. For most starches, however,
pastification does not commence below 70 C. (158 F.)
Classification. Commercial starches are classified, according
to the viscosity of the paste produced, as thick- or thin-boiling.
Wheat starch is a typical thin-boiling starch, as a 5% mixture
of wheat starch in water yields a thin, translucent syrup, scarcely
gelatinous at boiling temperature. Corn starch, on the other
hand, is a characteristic thick-boiling starch. Its 5% mixture
with boiling water is practically non-fluid.
While it is now known that variations in the pasting quali-
ties of a variety of starch can be induced by changes in the con-
ditions of manufacture or by suitable treatments, these properties
as well as the degree of gelatinization of the cooled paste are
of great importance to many industries. In laundry practice and
some branches of textile manufacture, for instance, it is essential
that the starch paste be thin enough to penetrate the fabric when
hot, without piling up on the surface, and at the same time that
it have body enough to provide the necessary stiffness to the
STARCH 9
finished article. On the other hand, in paper-box making, to
cite one example, a thick-boiling starch which will be adhesive
without soaking into the stock is required.
In the fermentation industry the pasting qualities of a starch
are only of minor importance since adaptations can always be
made to provide for them. The essential value of starch to
the fermentation industry is that by suitable treatment it yields
progressively more soluble products and finally can yield almost
100% of dextrose.
Conversion. The conversion of starch results first in the so-
called soluble starches, then in dextrin, then in maltose and
finally in dextrose. The earlier stages of the process are not
sharply defined from a chemical point of view and they are con-
trolled entirely with a view to the special qualities desired in the
product. As the conversion continues, mixtures of an unfer-
mentable gum, dextrin, with varying proportions of maltose and
dextrose are obtained. By carrying the process further, a yield
of almost pure dextrose can be secured. This, of course, is the
object in the processing of starch for the fermentation industry.
The conversion of starch results either by the action of the
enzyme, diastase, by boiling with dilute acids or by gentle roast-
ing. The first two methods are used in the fermentation industry,
often in conjunction with each other.
Chemically the process is a hydrolysis. That is, by the addi-
tion of water to the starch molecules, the latter are split into
more soluble materials. The products obtained depend upon
the agent used, and, also, upon whether the action is allowed
to go to completion. Many researches have been made in the
study of this subject. C. O'Sullivan (J.C.S. 1872, 579; 1876,
725), showed that the products of diastatic action are maltose
and dextrin, and that the proportion of maltose in the product
decreases as the temperature of conversion is raised above 63 C.
According to Brown, Heron and Morris (J.C.S. 1879, 596],
malt extract at room temperature converts starch paste into 80.9
parts of maltose and 19.1 parts of dextrin, and the same change
occurs at all temperatures to 6oC. The intermediate dextrins
were investigated by Brown and Morris (J.C.S. 1885, 527;
io SUGARS AND STARCH
1889, 449) 462], and by Brown and Miller (J.C.S. 1889, 286).
Various views have been held as to the nature of the intermediate
products, and even of the final products. Daish (J.C.S. 1914,
105, 2053, 2065} and Nanji and Beazley (J.S.C. Ind., 1926,
2/57*), state that prolonged treatment with mineral acid con-
verts starch into dextrins and maltose and finally into d-glucose.
Ordinary diastase, or amylase, a /^-diastase, converts starch
finally into dextrins and maltose, whereas takadiastase. which
contains the enzyme maltase in addition to an a-diastase, yields
J-glucose as final product. (Davis and Daish, B. C. Abs. 1914,
ii, 588. Cf. Baker and Hulton, J.C.S. 1914, 705, 1529; W. A.
Davis, J. S. Dyers, 1914, 30, 249}. G. W. Rolfe (Rogers 1
Manual of Industrial Chemistry, 1921, go 5-906} states that since
the discovery of the process of converting starch into dextrose by
the action of heat and acids, dextrose in a crude form and known
as starch sugar or grape sugar has entered into commerce, more
or less. There is also a very pure dextrose commercially sold
under the name "Cerelose." Its importance is small, however,
as compared to that of Commercial glucose. " He draws atten-
tion to the fact that there is some confusion of terms which as-
sociate this starch product with grape sugar and dextrose. It is
quite true that dextrose (^/-glucose) is an ingredient of commercial
glucose, but the dextrose in the commercial glucose of today is
the least important ingredient, both in quantity and for the quali-
ties which it imparts to the product. He gives a diagram (See
Figure I ) which shows the variation in proportion of the three
primary constituents of commercial glucose; dextrin, maltose,
and dextrose, present as acid hydrolysis of the carbohydrate mat-
ter proceeds. The progress of the hydrolysis is shown by the
change in optical rotation from that of starch paste to that of
dextrose. The diagonal dotted lines show the respective dextrin
and maltose percentages obtained in starch products hydrolyzed
by diastase (malt) conversion for the corresponding rotation
values. /These are corrected for the polarization influence of
carbohydrates introduced in the malt, which do not come from
starch hydrolysis. He states, further, that the stage of hydroly-
sis most favorable for the manufacture of commercial glucose
STARCH ii
for ordinary purposes lies between the rotation values, 120 and
140, although glucose used for special brewing purposes may
be somewhat outside these limits.
Maquenne and Roux (C.R., 1905, 140, 1303], claim that
starch is a mixture of two substances, amylose and amylopectin,
the former in the interior portion of the granule, and the latter
in the envelope. The amylose, obtained by reversion, or by
heating starch with water under pressure and cooling, gives no
Commercial Glucose
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FIG. i.
coloration with iodine in the solid state, is not readily attacked
by diastase, and is scarcely soluble in water at 120 C. If, how-
ever, it is heated with water under pressure at 150 C. it dis-
solves fairly readily; the solution can be filtered, gives a blue
coloration with iodine and is completely converted into maltose
by malt extract at 56 C. It is probable that the amylose and
amylopectin are not homogeneous (C.R. 1908, 146, 542). Schry-
ver and Thomas (Bio. J., 1923, 77, 497)1 have found that cer-
tain starches contain small amounts of hemicelluloses, and Ling
12 SUGARS AND STARCH
and Nanji (J.C.S. 1923, 725, 2666), state the ratio of amylose
to amylopectin is constant and is equal to 2:1, although their
absolute percentage will vary according to the proportion of
hemicellulose in the starch. For practical purposes, the progress
of the hydrolysis or conversion of starch paste is shown by char-
acteristic chemical and physical changes. The thick paste loses
its colloidal nature and rapidly becomes more limpid, the con-
centration (e.g., osmotic pressure) of the solution increases,
although the dissolved carbohydrates become specifically lighter,
and the solution becomes distinctly sweeter in taste. If tested
with a weak aqueous solution of iodine, the deep sapphire blue
given by the original starch paste changes as the hydrolysis pro-
ceeds, passing into violet, then to a rose red which in turn
changes to a reddish brown which grows steadily lighter, until
just before complete hydrolysis is reached, it disappears alto-
gether. A few drops of the solution poured into strong alcohol
give a copious white precipitate during the early stages of the
conversion; as the hydrolysis continues the amount of the precipi-
tate becomes less until near the end when no precipitate is
produced.
If the conversion products are tested polariscopically, it will
be found that there will be a progressive fall in specific rotation
values from that of starch paste (202) to that of dextrose
(52.7). The Fehling test shows no copper reduction with
starch paste, at the beginning of the hydrolysis, but progressively
increases till the maximum reducing power is reached when all
of the converted products are finally transformed into dextrose.
CHAPTER II
THEORETICAL CONSIDERATIONS. ENZYMES
At the beginning of the preceding chapter the statement was
made that fermentation results from the action of living bodies
on suitable organic compounds. The actual instruments of the
conversion, however, are not living cells but constitute a group of
special chemical compounds which are built up or secreted by the
living cells and which are called enzymes. We know that these
enzymes are not living bodies because the changes which they
produce can be effected in the entire absence of any live cells.
Yeast juice, for example, even when totally free of yeast cells
can cause the fermentation of suitable sugar solutions. The ac-
tivity of the juice diminishes in the course of time, and both in
rate of fermentation and in total fermentation produced; the
extract or juice is much less efficient than an equivalent amount
of living yeast.
Description. As a class, the enzymes are unstable, nitrog-
enous compounds of a colloidal nature and of great chemical
complexity. Only t\vo enzymes, urease and pepsin, have been
isolated in a fairly pure state. The exact chemical composition
of the enzymes is still unknown. They are not necessarily pro-
teins although many of them have certain properties common to
proteins. Their most important characteristic is the ability to
produce chemical changes in other substances without themselves
being changed. This is what chemistflf s call catalytic power. An-
other name for the enzymes as a group is chemical or soluble
ferments.
Specific Action. When enzymes are considered separately
rather than as a class it is found that their individuality manifests
itself in two ways; a combination of one special enzyme with one
special substrate (material to work on) is required for each par-
13
14 ENZYMES
ticular result. However, it is possible to classify enzymes to
some extent by the type of reaction which they produce, as
follows :
GROUP ACTION
1. Hydroxylases Invertase hydrolyses cane sugar. Amylase
hydrolyses starch.
2. Esterases Hydrolyse esters, including the lipases which
act specifically on fats.
3. Oxidases Produce oxidation.
4. Reductases Produce reduction as e.g. reduce aldehydes to
alcohol.
^5. Carboxylases Split off carbon dioxide from organic acids.
6. Clotting enzymes Thrombase, which clots blood. Rennin, which
clots milks.
It is now customary to name enzymes after the compound on
which they act with the addition of the ending "ase."
There are also known some cases in which enzymes tend to
prevent rather than produce a reaction. In the majority of cases
their action as catalysts is positive. That the action is truly
catalytic is shown by the fact that the rate of reaction is directly
proportional to the concentration of the enzymes, but the total
amount of action is independent of the amount of enzyme,
provided a sufficient time is allowed; and provided also that the
enzyme is not decomposed by other means. As a rule a small
amount of enzyme cannot decompose unlimited amounts of sub-
strate, since most enzymes are relatively unstable. Hence, if only
a small amount of enzyme is used the reaction slackens and
finally ceases, owing to decomposition (autolysis) of the enzyme
before all the substrate has reacted.
Conditions of Functioning. Enzymes are sensitive to high
temperatures, e.g. y when heated to below 100 C. their activity
is completely destroyed. They are, however, resistant to many
antiseptics which destroy protoplasm and kill fermenting organ-
isms. Some germicides, such as formaldehyde, tend to destroy
, enzymes.
1 Preparation. Enzymes are concentrated by precipitation
from their solutions by the addition of alcohol or acetone, or by
SELECTIVITY 15
the addition of salts such as ammonium sulphate; by precipitation
after adjustment of the solution to a definite pH; or by adsorp-
tion by such materials as alumina, silica gel, fullers' earth, etc.
Often combinations of these procedures are used. The resulting
products, however, are often contaminated with other enzymes
and with inactive impurities, all of which makes the study of their
reactions difficult.
Selectivity. The action of enzymes is essentially selective,
in this respect differing from the action of inorganic catalytic
agents. The following tabular representation of the reactions of
the trisaccharide, raffinose, will illustrate this:
SUGAR CATALYST PRODUCTS
Raffinose Acid Dextrose, fructose, galactose
Raffinose Diastase Melibiose, fructose
Raffinose Emulsin Galactose, sucrose
In general, esters, amides, carbohydrates, glucosides, etc. are
all hydrolyzed by hydrochloric acid. Lipases will hydrolyze es-
ters but not carbohydrates. Maltase will hydrolyze maltose but
not sucrose. Even slight differences in the configuration of two
sugars will be sufficient to affect their reactivity with a particular
enzyme.
It will be seen that the activities of the hydrolytic enzymes
are so specific that great care must be exercised to provide those
enzymes which, working on the available materials, will produce
the desired results. While this circumstance is of great theo-
retical importance, it enters into practical consideration rather
rarely. As a rule each naturally occurring saccharide or other
hydrolyzablc substance is accompanied by its own specific hydro-
lytic enzyme so that it can be made available for natural utiliza-
tion. The enzyme does not necessarily exist as such in the tissue,
but may be present as a so-called zymogen, which liberates the
enzyme under suitable conditions, such as a wound to the organ-
ism or the presence of an acid.
Co-enzymes. Very often also there are required the pres-
ence of two factors, the enzyme and the co-enzyme to produce
the fermentation. For example, it has been shown by Harden
1 6 ALCOHOL-PRODUCING ENZYMES
and Young (J.C.S. 1905 Abs. II; iog and ibid. 1906, I; 470)
that yeast juice can be separated by dialysis into two fractions
which when recombined are equal in activity to the original juice,
although neither by itself will cause any fermentation. The
dialyzable fraction, the co-enzyme, is resistant to boiling, but dis-
appears from yeast juice during fermentation, or when the juice
is allowed to undergo autolysis. It is decomposed by acid or
alkaline hydrolyzing agents, by repeated boiling, and by the lipase
of castor beans. The presence of both an enzyme and a co-
enzyme has been found necessary in other fermentations, e.g., in
the action of lipase it has been found that a co-enzyme which is a
salt of a complex taurocholic acid is required.
Alcohol-producing Enzymes. As can be inferred from the
above, the number of types of enzymes required to carry on a
practical fermentation may vary from one to three or more, ac-
cording to the substrate to be fermented.
Zymase, which carries on the final conversion of the mono-
saccharide to alcohol and carbon dioxide in accordance with the
chemical equation:
Dextrose (or fructose, etc.) Alcohol Carbon Dioxide
C 6 H 12 O 6 ^ 2C 2 H 5 OH + aCO 2
is always necessary.
A hydroxylase such as maltase or invertase is usually needed
to convert maltose or sucrose respectively into mono-saccharide
sugar. This conversion follows the formulation
Disaccharide (Sucrose, Water Hexoses (Dextrose,
maltose, etc.) fructose, etc.)
CigH^Oii + H 2 O i CgH^Og + CgH 12 O6
Finally another enzyme may be needed to saccharify, i.e.,
hydrolyze, the starch into maltose. Successful fermentation de-
pends very largely upon the supplying of the required enzymes at
the proper stage in the operation, and in the necessary amount to
produce the desired result. Further consideration of these topics
will be found under the captions of Yeast and Malt.
CHAPTER III
THEORETICAL CONSIDERATIONS. FER-
MENTATION
Alcoholic fermentation is a subject which has attracted the
study of many chemists, even some of the greatest. Many days
of research have been devoted to define completely the reactions
which take place in this chemical transformation, and various
theories have been advanced to explain the steps which occur.
Despite all this work, our knowledge of its mechanism is still in-
complete. We know that fermentation commences with sugars
in the presence of certain other materials, ferments or enzymes;
and we know most of the end products. But we do not know
how these products result, why they result, or what are the inter-
mediate steps in their formation. A completely satisfactory
explanation still has not been found in answer to these questions.
General Requirements. Sugar, water, the presence of a fer-
ment, and a favorable temperature, usually 75 F.-85 F. and
never over 90 F. are inescapable requirements. There are other
limiting factors. The ferments or enzymes are known to be
chemical compounds. They have not been analyzed completely,
however, nor synthesized, and we are dependent for their pro-
duction upon living plants, the yeasts. The reactions follow the
law of Mass Action to the extent that as the concentration of the
alcoEol approaches 14-16% the reaction slows down and finally
stops. The law of Mass Action states that in a reversible reac-
tion the final state reached depends on the relation between the
concentrations of the initial and end materials. However, at-
tempts to reverse the process of fermentation have been successful
only in the minutest degree.
Oxygen does not appear to enter into the fermentation
reaction, but the presence of air and particularly aeration of the
fermenting liquor, the substrate, do have a noticeable influence.
17
1 8 FERMENTATION
Essential Nature. Whatever the starting point, in all cases
the desired result is the presence of all of the sugars in a form
suitable for conversion into alcohol. As previously stated, this
process is called alcoholic fermentation. This change was be-
lieved by Lavoisier (1789) to follow the formulation:
C 6 H 12 O 6 = 2C 2 H 5 OH + 2C0 2
Hexose Ethyl Alcohol Carbon Dioxide
It was shown by Pasteur (1857) ^at this formulation actually
accounts only for about 95% of the sugar consumed. Glycerin,
organic acids and traces of other by-products account for the
balance. This figure of 95%, however, does represent the yield
of alcohol which is obtainable under favorable conditions and
represents also the upper limit of the result of good commercial
practice in the production of alcohol, either potable or industrial.
Since their time, the combined labors of many students have,
on the one hand, added somewhat to our knowledge of the
mechanism of fermentation; and on the other hand, have de-
fined some of the by-products as well as some of the minor
prerequisites to success.
Products. Pasteur found that the actual yield from the fer-
mentation of 100 pounds of sugar was as follows:
Alcohol .............................. 48.55 Ib.
Carbon Dioxide ....................... 46.74 Ib.
Glycerol ............................. 3.23 Ib.
Organic Acids ........................ 0.62 Ib.
Miscellaneous ......................... 1.23 Ib.
100.37 H>-
The fact that the total weight of fermentation products ex-
ceeds slightly the weight of sugar fermented is explained by the
absorption and fixation of small amounts of water to make cer-
tain of the by-products. According to Pasteur some sugar is
also utilized by the yeasts in building new yeast cells.
In general, the chief products of vinous fermentation may be
stated to be: alcohol and carbon dioxide (accounting for 94-95%
of the sugar), glycerol 2.5-3.6%, acids 0.4-0.7%, and, in addition,
CONTROLLING FACTORS 19
an appreciable quantity of fusel oil (higher alcohols), some
acetaldehyde and other aldehydes and some esters. Among the
minor products of fermentation maybe listed the following which
have been identified:
Formic Acid
Acetic Acid
Propionic Acid
Butyric Acid
Lactic Acid
Ethyl Butyrate
Ethyl Acetate
Ethyl Caproate, etc.
Rate of Fermentation. The ratio of carbon dioxide to al-
cohol produced and the ratio of yeast formed to alcohol produced
both vary at different stages of the fermentation. They depend
both on the age of the yeast and on the age of the fermentation.
Slator, J.C.S. (1906), 89; 128, and ibid. (1908), 93; 217 has
shown that the rate of conversion of dextrose into alcohol and
carbon dioxide by yeast is exactly proportional to the amount of
yeast present and, with the exception of very dilute solutions, is
almost independent of the concentration of sugar. Slator and
Sand, Trans. Ch. Soc. (1910) 97; 922-927 have further de-
veloped and explained this fact by showing that the diffusion of
sugar into the yeast cell is so rapid even in dilute solutions that
more sugar is present in the cell than can be fermented at any
instant. Various yeasts will ferment levulose (fructose) at the
same rate as that at which dextrose is fermented. Similarly,
maltase-containing-yeasts will ferment maltose solutions at the
same rate as if dextrose were being fermented.
Controlling Factors. The factors which really govern the
rate of fermentation, then, are two: the concentration of yeast
and the temperature. The latter is of the greatest importance.
Taking as a unit the amount of fermentation produced at 32 F.,
six times as much will result in the same time at 77 F., and
twelve times as much at 95 F. However, the rates of forma-
tion of undesired by-products and of autolysis of the yeast also
increase objectionably as the temperature is raised, hence it is
20 FERMENTATION
usual to set an upper limit of 90 F. on the fermentation. Since
heat is evolved during the process, this requires that the rate
must be so controlled that either natural radiation or artificial
cooling will keep the temperature within the desired limits.
Inorganic Requirements. Various inorganic constituents
must also be present in the fermenting liquor. Some of these,
phosphates in particular, play a part in the mechanism of fer-
mentation. Others are necessary to provide food for the yeast,
nitrogen compounds, calcium, potassium and manganese, etc. In
addition there is a still incompletely defined compound called
"bios" which appears to be essential to success. Most of these
are present in sufficient amounts in the raw materials of the fer-
mentation industry although it is probable that close study of their
occurrence might be rewarded by increased yields and/or im-
proved products.
Mechanism. The role of phosphates especially is of interest
since it shows that the fermentation proceeds by steps instead of
immediately in the sense of the equation
C 6 H 12 O 6 z^2C 2 H 5 OH 4- 2CO 2
Harden and Young, J. Ch. Soc. (1908) Abs. i, 590 were the first
to show that the addition of phosphates (disodium phosphate) to
a mixture of yeast juice and dextrose resulted in both an initial
acceleration and in an increased total fermentation. They also
showed that there was an optimum concentration of phosphate,
deviations from which in either direction resulted in a diminished
rate of fermentation. It is assumed that a hexose-di-phosphate
is formed as follows:
C 6 H 12 O 6 + 2Na 2 HPO 4 -> C 6 H 10 O 4 (PO 4 Na 2 ) 2 + aH 2 O
It is this compound which breaks down into alcohol and carbon
dioxide and regenerates the sodium phosphate. The latter can
then again combine repeatedly with the sugar, sensitizing it to
the breaking down action of the enzyme until the fermentation
is complete. It has been shown by careful experiments that dur-
ing the period of increased fermentation the amounts of alcohol
and carbon dioxide produced are stachimetrically related to the
MECHANISM 21
quantity of added phosphate in the ratio C 2 H 5 OH : Na 2 HPO 4 .
Since the filtered enzyme plus phosphate will not of themselves
induce fermentation, it follows that phosphate is not the co-
enzyme. On the other hand, in the entire absence of phosphate
no fermentation occurs even though both enzyme and co-enzyme
are present. Arsenites and arsenates cause some acceleration of
the fermentation, but they cannot be used in place of phosphates.
They appear rather to act as accelerators in the decomposition of
the dextrose phosphate.
It has been found by further investigation that there is ap-
parently another step in the fermentation reaction in which the
dextrose di-phosphate splits into two moles of triose mono-phos-
phate. It should be particularly noted that the immediately
preceding study of the mechanism of the action of yeast juice is
not directly applicable to the action of yeast. E.g. } Slator (loc.
cit.) found that phosphates are without accelerating effect when
living yeast cells are employed.
Many other suggestions have been made regarding the inter-
mediate steps in the conversion of dextrose into alcohol and
carbon-dioxide and the nature of the intermediate products.
Biichner and Meisenheimer, B. (1905), 38; 620, suggested that
lactic acid is the first product of the action of zymase on dextrose
since it is known that this acid is formed in muscle tissue by the
oxidation of glycogen, which is a polydextrose. They added to
this theory the assumption of a second enzyme, lactacidase, which
carries on the decomposition of the lactic acid into ethyl alcohol
and carbon dioxide; cf. Bio. Z. (1922), 128 ; 144 and 132 ; 165.
This suggestion was based on the observation that a concentrated
solution of dextrose when treated with alkali yields about 3%
of alcohol on exposure to sunlight. Under similar conditions a
more dilute solution gives a 50% yield of lactic acid.
Another suggestion is that dihydroxy-acetone, CO(CH2OH) 2
is the first result of the splitting of the hexose molecule. It has
been shown by Biichner and Meisenheimer, B. 43; 1773 and by
Lebedew, B., 44; 2932. Cf. also Franzen and Steppuhn, ibid.,
2915 that dihydroxy-acetone is fermentable by yeast. It has also
been shown that dihydroxy-acetone and glyceraldehyde can, under
22 FERMENTATION
suitable conditions be condensed to form a hexose so that there
is every probability that the reaction is reversible. Again, the
suggestion has been made that glyceraldehyde, C(HO)'
C(HOH) C(H2OH), by the loss of water yields an enolic
compound CH : C(OH) CHO called methyl-glyoxal ; which, by
the addition of water can yield either lactic acid or even ethyl
alcohol and water. On the other hand, the above mechanisms,
although plausible, appear improbable as important parts of the
fermentation reaction since it has also been shown that glycer-
aldehyde is only slowly fermented while methyl-glyoxal and lactic
acid are unacted upon by yeast juice or yeast.
Neuberg, Deut. Zuckerind. (1920) 45, 492, has shown that
yeast contains an enzyme, carboxylase, which is capable of elimi-
nating carbon dioxide from a-ketonic acids, and therefore suggests
that pyruvic acid CH 3 CO COOH represents the initial splitting
product of fermenting hexose. The reaction, then, proceeds with
the decomposition of the pyruvic acid into acetaldehyde and car-
bon dioxide, and the aldehyde is reduced by the yeast to ethyl alco-
hol. In support of this theory it has been shown that the addition
of pyruvic acid to a fermenting liquor increases the yield of alco-
hol. The presence of glycerol, which may function merely as a
yeast preservative, is required. It is also known that there is pres-
ent in yeast an enzyme which is capable of reducing aldehyde.
However, the conversion of the hexose into pyruvic acid is diffi-
cult to formulate logically.
Neuberg and Arinstein, Bio. Z. (1921), 117; 269 and 122;
suggest the following steps for the fermentation:
1 i ) Dextrose ^ Water + Methyl-Glyoxal-Aldol
C 6 H 12 O 6 ^ aH 2 O + CH 3 CO CH(OH) CH 2 CO - CHO
This keto form changes to the enol-form
CH 2 : C(OH)- CH(OH) CH 2 CO CHO
(2) Methyl-Glyoxal-Aldol ( keto form ) + Water ^
Glycerol 4- Pyruvic Acid
CH 2 :C(OH)-CH(OH) CH 2 CO-CHO + aHO^
CH 2 (OH) CH(OH) CH 2 (OH) + CH 3 CO COOH
BY-PRODUCTS 23
Part of the pyruvic acid is converted by the action of carboxylase and
reductase into alcohol and carbon dioxide.
(3) Methyl Glyoxal + Acetaldehyde + Water ^
Alcohol + Pyruvic Acid
CH 3 CO CH : O + CH 3 CHO + HoO ^
CH 3 CH 2 (OH) + CH 3 CO COOH
In support of this exposition Neuberg cites the three different
courses taken by the fermentation according to conditions :
(a) Normal in fairly acid media with over 90% yields
C 6 H 12 O 6 - 2C 2 H 5 OH -f 2CO 2
(b) In the presence of sulphites (to fix aldehyde)
C 6 H 12 6 - C 3 H 5 (OH) 3 + CH 3 CHO + CO 2
(c) In faintly alkaline conditions (in the presence of sodium bicar-
bonate)
2C 6 H 12 6 +H 2 - 2C 3 H 5 (OH) 3
-f 2CO 2 + C 2 H 5 OH + CH 3 CO 2 H
In reply to the objection that acetaldehyde and pyruvic acid are
not so readily fermentable as dextrose, Neuberg suggests that the
reaction takes place with one of their tautomeric (enolic) forms.
By-products. Glycerol. The preceding formulations of the
fermentation reaction indicate readily the production of glycerol.
Biichner and Meisenheimer have shown that it is formed in sugar
solutions even by the action of yeast juice without the require-
ment of living yeast cells. It is known also that by the addition
of sodium carbonate or sulphite and by selection of the most
suitable yeasts a yield of 25% or more of glycerol on the weight
of sugar fermented can be obtained.
Fusel Oil and Succinic Add, etc. It has been shown that this
group of by-products derives not from the sugar but from other
materials present in the fermenting liquor. F. Ehrlich in many
researches (1904-1910) has shown that the higher alcohols and
aldehydes, which when mixed we call fusel oil, are formed by the
deammination of amino acids resulting from the hydrolysis of
proteins. Thus isoamyl alcohol, which is the chief constituent of
fusel oil, is closely related to leucine, amino-isohexoic acid, and
active amyl alcohol is similarly related to isoleucine, a~amino-/3-
24 FERMENTATION
methyl-valeric acid. Both of these acids are formed in the
hydrolysis of proteins and both, according to Ehrlich, are trans-
formed into the corresponding amyl alcohols in the presence of
sugar by the action of pure yeast cultures. The gross reaction is
formulated as follows:
(CH 3 ) 2 CH CH 2 - CH(NH 2 )- COOH + H 2 O
(CH 3 ) 2 CH CH 2 CH 2 (OH) + CO 2 + NH 3
In a similar manner the other amino acids react; tyrosine, /?-p-
hydroxy-phenyl-a-amino-butyric acid yielding p-hydroxy-phenyl-
ethyl alcohol, tyrosol; while phenyl-alanine, a-amino-/?-phenyl-
propionic acid, yields phenyl-ethyl alcohol. Succinic acid, for ex-
ample, which is of usual occurrence in fermented liquors is
probably formed by a similar reaction from glutamic acid with the
additional step of oxidation in the process.
These changes take place only by the action of yeast but not
by the action of yeast juice. This fact points to the importance
of these reactions in the life process of the yeast cell. A similar
conclusion results from the fact that no free ammonia is found
at the end of the reaction, all of it having been consumed in the
building up of new yeast cells. This conclusion is further
strengthened by the fact, also shown by Ehrlich, that if appre-
ciable amounts of simple nitrogenous bodies, such as ammonium
salts, are present in the fermenting liquor these will be used by the
organisms in preference to decomposing the amino-acids. Ehrlich
has found it possible to increase or diminish the amounts of
fusel oil formed by diminishing or increasing the amounts of
ammonium salt added to the wort; and also to increase the yield
of fusel oil by adding larger amounts of amino-acids to the fer-
menting mixture. Practically all amino-acids formed in the
hydrolysis of proteins can be similarly decomposed by yeast cells
provided that sugar is present. As previously stated enormous
amounts of research have been devoted to the mechanism of the
fermentation reaction. Despite this, the complete definition of
the reaction has not been arrived at. The point of interest here
is that there are a large number of factors involved, many of
them known and controllable and necessary to success.
CHAPTER IV
THEORETICAL CONSIDERATIONS. RAW
MATERIALS
General Classification. The preceding chapters have been
devoted to a brief discussion of the chemical background which
is common to all of the fermentation industry. The various raw
materials which, by the application of the principles developed,
are converted into alcohol-containing beverages will be discussed
in the present chapter. The diversity of these raw materials is
very great, since anything which contains sugar or may be treated
to yield sugar, will serve and probably has been applied, to pro-
duce intoxicating liquor. It is possible to classify these materials,
therefore, in two ways. However any classification may err at
times as industrial demands change. The classification may be :
I. According to their function as sugar suppliers or auxiliaries.
II. According to the products into which they enter.
On the first basis we find three groups:
A. Materials which supply preformed sugar for fermentation.
Fruit and fruit juices
Molasses
Honey
Sugar, etc.
B. Starch-containing materials yielding fermentable sugar on treatment.
Cereal grains
Potatoes, etc.
C. Auxiliary materials which contribute neither sugar nor starch.
Spices and other Flavoring matters
Coloring Agents
Blending Agents, etc.
This classification is based on applicability or composition.
On the basis of use the same materials may be reclassified:
26 RAW MATERIALS
A. Materials for the production of distilled spirits.
Cereal grains
Potatoes
Molasses
Flavoring and Coloring Agents, etc.
B. Materials for the production of wines.
Fruit juices and fruits
Sugar, etc.
C. Materials for the production of liqueurs and cordials.
Alcohol
Sugar
Spices and Essential Oils
Coloring Agents, etc.
Distilled Spirits. The materials used for the production of
distilled spirits are further classified according to the types of
product in which they find employment:
American Whiskies
Rye
Barley
Rye
Bourbon
Barley
Corn
Wheat
Scotch Whiskies
Pot Still Type
Barley
Patent Still Type
Barley
Rye
Corn
Oats
Irish Whiskies
Pot Still Type
Barley
Rye
Oats
Wheat
DISTILLED SPIRITS 27
Patent Still Type
Barley
Rye
Corn
Oats
Gin (Distilled)
Barley
Rye
Corn
Kornbranntwein
Barley
Rye
Corn
Wheat
Vodka
Barley
Rye
Corn (In cheaper grades)
Rum
Molasses
Cane Juice
Schnapps
Potatoes
Brandy
Grape juice and marc.
Other fruits (Apples, prunes, cherries, etc.)
Since the entire spirit industry is designed to produce palatable
products, the tabulation given above is not necessarily binding.
Some of the materials listed are very seldom used. Practice may
differ from plant to plant producing the same product or may be
influenced from year to year by changed crop and economic con-
ditions. Owing to the great variety of distilled liquors in flavor
and general character, and the influence on these of both the
materials used and the processes by which they are treated, it
is impossible to be completely general. However, it may be stated
that the important cereal grains to the liquor industry are in
order: barley, rye, corn, oats, and wheat. A short discussion
of these grains including both their botanical and chemical char-
acteristics follows:
28
RAW MATERIALS
Cereal Grains. Barley. Barley takes the first place in im-
portance in the spirit industry on account of its high production
of the enzyme, diastase, when permitted to sprout (malt). There
are several types of barley which are largely used. These include :
1 i ) a. Hordeum distichum, a two-row type which includes the well-
known varieties Chevalier, Hallett, Hanna.
b. Hordeum zeocritum, two-row fan-shaped barleys of which
Goldthorpe is the leading variety.
(2) Hordeum vulgare, the ordinary six-row barley, such as Manchu-
rian, Oderbrucker, Scotch, etc.
(3) Hordeum hexastichum, which likewise have their flowers on a
spikelet fertile, but on account of the fact that the ears are wide,
the appearance of the head is a hexagon when examined from the
top. These are really six-row barleys. An example of these is
the white barley of Utah and adjoining States.
The average composition of barleys of these three types, to-
gether with data as to weight, are given in the following
tabulation :
TABLE I. AVERAGE PERCENTAGE COMPOSITION OF THREE TYPES OF
MALTING BARLEYS (LE CLERC) *
Type of barley
Mois-
ture,
Water-free basis
Wt.
per
bushel,
pounds
Wt.
per
1,000
grains,
grams
Ash,
/o
Pro-
tein,
Fat,
Fiber,
Pento-
sans,
Starch
Two-row
8. 9
8. 7
2 . Q
3-0
2. 9
ii. 6
11.9
IO.O
2.0
2.0
2.0
5-*
5.8
8-4
9.6
9.0
59.1
58.9
59-9
5*
47
48
38
27
38
Ordinary six-row
Hexastichum
i U. S. Dept. Agr., Bureau of Chemistry. Bull. 124, Le Clerc and Wahl, Chemical studies of
American barleys and malts.
The two-row barleys are chiefly grown in Europe, although
they are raised in this country in Montana, Idaho, New York,
etc., to a limited extent. On account of their relatively high car-
bohydrate content and low protein, they are particularly adapted
to use in the brewery.
CEREAL GRAINS 29
In this country, the ordinary six-row barley is the kind most
abundantly produced, being raised extensively in the States of
the Mississippi Valley. Its relatively high protein content causes
it to produce malt of high diastatic power, and thus fits it espe-
cially to use in the distillery.
A good distiller's barley should be free of dirt and have good
odor and color, small grains of uniform size, a high percentage
of nitrogen, and high germinating capacity. With these charac-
teristics and with proper treatment in the malt house, it is bound
to yield a malt of good character.
Cleanliness is necessary, not only because dirt is not a source
of alcohol, but because it is sure to carry large numbers of bac-
teria and molds, which interfere with the production of a good
malt.
Barley is composed of about 12 per cent husks, 10 per cent
bran, 2.5 per cent embryo, and the rest endosperm or the stored
food for the plantlet. The husks and bran are merely protective.
The germ is the seat of life; it consists of embryonic radicles or
rootlets and the plumula or acrospire. The sprouting of this
germ is essential to the production of malt since this serves to
convert the starch of the endosperm into fermentable sugar. The
endosperm is composed mostly of starch and protein, but both
of these substances are insoluble and non-diffusible and can not
be used directly in supplying food for the young plant. The
agency which renders these soluble and diffusible is an enzyme
or a series of enzymes secreted by the embryo during growth,
one of which, the diastase, dissolves the starch and converts it
into sugar and dextrin, while another, the peptase, acts on the
protein. These enzymes are developed in the growing malt as
the germ's need for food increases. The products of enzyme
action are soluble and diffusible, and can be directly used as food
by the growing embryo.
Barley contains about 65 per cent of fermentable matter;
and at a weight of 48 pounds per bushel one ton should produce
about 98 gallons of alcohol.
Barley, to be considered good, should show a germination
of at least 97 per cent. If below this limit of vitality, it should
30 RAW MATERIALS
be reduced in price, or rejected. Grains which are incapable of
germination are not only useless, but harmful, because they act
as carriers of micro-organisms which may infect the rest of the
grain.
Rye. Rye is, comparatively speaking, a minor crop in the
United States. The only species under cultivation is the common
rye : Secale cereale.
In structure and habits of growth, rye resembles wheat, and,
like wheat, it is grown as both a spring and winter crop. It is
a tall-growing, annual grass with fibrous roots, flat, narrow, bluish-
green leaves, standing erect or decurved and having slender cylin-
drical spikes consisting of two or three-flowered spikelets. The
flowering glumes are long-awned or bearded and lance-shaped,
and are so firmly attached that little chaff results from the thresh-
ing. The individual grains are partly exposed and are longer,
more slender and more pointed than wheat. They are dark,
with a slightly wrinkled surface and are very hard and tough,
requiring more power to mill than any other grain.
The following is an analysis of common rye :
TABLE II
Moisture 1 1 . o%
Ash 2.0%
Protein (N X 6.25) n.6%
Ether extract i . 7%
Crude fiber 2.0%
Pentosans 8.5%
Total sugar 4 . o%
Other carbohydrates 59. 2%
Wt. per 1,000 grains 25.0 grams
Wt. per bushel 56.0 Ibs.
Rye is very largely used in distilleries which produce potable
spirit such as whiskey, gin and vodka, and in the manufacture of
compressed yeast It is also used in relatively small amounts in
the yeast mashes of alcohol distilleries. It is not suited to use as
the chief ingredient of the mash in an alcohol distillery, on ac-
count of the tenacious quality of the mash which it forms. Fur-
thermore, it gives a low yield in proportion to the amount of
starch which it contains. Though it usually contains over 60
CEREAL GRAINS 31
per cent of fermentable matters, it rarely produces over 85 gal-
lons of alcohol to the ton.
Corn. This valuable food stuff is the grain of a gigantic
grass known to botanists as Zea Mays. It originated in America
but subsequently was transplanted to many other countries, prin-
cipally France, Hungary, Italy, Spain, Portugal, South Africa and
Argentine.
There are over three hundred recognizable varieties, some
of which are only a few inches in height, while others are giants
of six feet or more ; some come to maturity in two months, while
others require three or four times as long before their cobs ripen.
There is also great variety in the shape, size, and color of the
actual grain. Some are white as, for example, the Cuzco maize,
others are yellow, red, purple, or even striped, and the varieties
differ among themselves in chemical composition.
The most important maize growing country of the world is
the United States. Many varieties are cultivated, but the chief
may be roughly grouped into four classes. First come the "Flint"
varieties which are most commonly met with east of Lake Erie
and north of Maryland, and the "Dent" varieties which are most
popular west and south of these localities. The "Horsetooth,"
which passes insensibly into the above forms, is grown chiefly in
the South. Lastly, the "Sweet" varieties are extensively cul-
tivated for the green grain. These are boiled and used as
a vegetable and seldom allowed to mature into the ripened
grain.
For the making of whiskey the finest white "Flint Corn" is
preferred. The Kentucky distilleries are extremely careful in
their selection of the raw material. Indian Corn that is grown
along the Ohio and the Kentucky Rivers is especially sought after
by the distillers as being peculiarly suitable. Corn which has been
injured by frost, heat, moisture or mold can readily be used in
the manufacture of industrial alcohol as such damage does not
affect the fermentable content of the grain and it can be bought at
a low price, but it is unsuitable for the liquor industry.
A typical American maize should have the following com-
position :
32 RAW MATERIALS
TABLE III
Weight of 100 kernels 38 grams
Moisture 10.75%
Proteids 10 %
Ether extract 4. 25%
Crude fiber 1 . 75%
Ash 1 . 50%
Carbohydrates other than crude fiber 71 .75%
Dry corn of good quality should yield at least 65% of sugars
and starch and should yield from 98 to 105 gallons of 180
alcohol per ton (shelled).
Oats. Oats is the grain or seed of the cereal grass Avena
sativa. It forms one of the most valuable sources of food for
both man and beast, the nutritive value of the grain being very
high. It is extensively grown in Great Britain, Continental
Europe, Russia and North America.
Practically four-fifths of the oat crop of the United States is
produced in the thirteen states extending from New York and
Pennsylvania westward to North Dakota, South Dakota,
Nebraska and Kansas. Each of these states devotes more than
a million acres to oats. The average yield in the six northern-
most states, New York, Michigan, Wisconsin, Minnesota, North
Dakota and South Dakota is 31.68 bushels per acre while their
total production is slightly less than one-third of the oat crop
of this country. The average yield of the other seven states,
Pennsylvania, Ohio, Indiana, Illinois, Iowa, Nebraska and Kan-
sas is only 29.23 bushels per acre yet they produce more than
half of the entire crop. The difference in yield of nearly two
and one-half bushels to the acre between these two groups of
states is due largely to the fact that the climatic conditions of
the northern group are better suited to the production of the crop.
There is no material difference in soil composition or other fac-
tors affecting the yield.
Oats are grown in the corn belt, which includes all the states
of the second group, largely because a small-grain crop is needed
in the rotation and because the grain is desired for feeding to
work stock. Spring wheat is seldom satisfactory in this district
and winter crops often do not fit well into a rotation which
CEREAL GRAINS 33
ordinarily includes corn, a small grain and grass. Under these
conditions oats are generally grown as the best crop between corn
and grass. This is particularly true in Illinois and Iowa, the
two states producing the greatest quantity of both corn and oats.
There are many factors which reduce the yield of oats in
the corn belt. In general, those varieties of oats which mature
earliest are best adapted to the belt, for early maturing often
enables a crop to escape hot weather, injury from storms, and
attacks of plant diseases. The early varieties also usually pro-
duce less straw and for that reason are less likely to lodge than
the ranker growing late varieties. A number of years ago the
Early Champion and the Fourth Qf July varieties came into
prominence but they are not now extensively grown, for, although
early in maturing, their yield is often unsatisfactory. Burt is a
very early variety much used for spring seeding south of the
Ohio River but little known elsewhere. The type of early oats
now most largely grown in this country is represented by the
Sixty-Day and the Kherson varieties, two comparatively recent
introductions from Europe.
The following is a typical analysis of a variety of oats:
TABLE IV
Moisture 1 1 . 6%
Ash 3.4%
Protein (N X 6.25) 1 1 . 5%
Ether extract 4 . 7%
Crude fiber n.o%
Pentosans 12.0%
Total sugar 1.5%
Other carbohydrates 44.3%
Wt. per 1,000 grains 29.2 grams
Wt. per bushel 32.0 Ibs.
This grain is not too well suited for distillery use because of
the glutinous nature of the mixture which is formed when it is
treated with hot water. It contains about 50 per cent of fer-
mentable substance and might be made to yield about 70 gallons
of alcohol per ton.
Wheat. Wheats have been cultivated by man since before
the dawn of history, and nothing is now known of the original
34 RAW MATERIALS
wild forms from which they are descended. In old legends and
ancient manuscripts wheat is spoken of as familiarly as at the
present day. Nor do we know with any certainly in which coun-
try it was first found; but it seems probable that Central Asia
was the original home of the wild forms from which the culti-
vated species have sprung.
Wheat belongs to the grass family, Pouceas (Germineae),
and to the tribe called Hordeae, in which the I to 8 flowered
spikelets are sessile and alternate on opposite sides of the rachis,
forming a true spike. Wheat is located in the subtribe Triticeae
and in the genus Triticum where the solitary two-to-many flow-
ered spikelets are placed sidewise against the curved channeled
joints of the rachis.
Great diversity is shown by the varieties of wheat grown in
the United States. More than 200 distinct varieties are grown.
Clark ("Classification of American Wheat Varieties" U. S. De-
partment of Agriculture, Dept. Bull. 1074, 1922) divides
American grown wheats into the following groups:
1 i ) Common
(2) Club
(3) Poulard
(4) Durum
(5) Emmer
(6) Spelt
(7) Polish
(8) Einkorn
(9) Unidentified
Within these groups are numerous types of which the follow-
ing more important are arranged in approximate order of pro-
duction and use:
Common
Turkey, Marquis, Fultz, Red Wave, Poole, Fulcaster.
Club
Hybrid (Grown only on Pacific coast)
Durum
In Dakotas and adjoining states
WINE MATERIALS 35
Emmer
Minnesota, Dakotas and adjoining states
Polish
New Mexico and Wyoming
(Not grown much)
Spelt
Not grown to any extent commercially.
The following is an analysis of two typical wheats:
TABLE V
Soft wheat Hard Wheat
Moisture.... = 12.0% 12.0%
Ash 1.9% 1.8%
Protein (N X 6.25) 9.0% 12.4%
Ether extract i.?% *-7%
Crude fiber 2.5% 2.5%
Pentosans 7-% 7-%
Total sugar 2.7% 2.7%
Other carbohydrates 63.2% 59-9%
Wt. per i, ooo grains 38. 7 grams 38.7 grams
Wt. per bushel 60.0 Ibs. 60.0 Ibs.
What has been said regarding the yield of alcohol to be
obtained from rye applies also to wheat and therefore, the latter
has not been much used in distilleries, even at times when it was
relatively cheap.
Wine Materials. The wine industry differs from the spirit
industry, among other things, in that the distinguishing character-
istics of the finished product, wine, are much more closely re-
lated to the individual character of the raw material. Although
almost all wines are made from grapes, the character of a single
batch of wine will depend not only on the variety of grape used,
but even on the special plot of ground on which it was grown and
the climatic conditions in the year of its growth. For this reason
a classification of materials for the wine industry in the same
manner as that given for the spirit industry is not possible. On
the other hand, a means of classification is possible based on the
geographical distribution of the grape varieties which are suc-
cessfully grown for wine production.
RAW MATERIALS
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WINE MATERIALS 37
Since the United States is geographically so large and offers
for grape culture at one spot or another every feature that can
he found elsewhere, the following tabulation and discussion is
confined to this country. The principles, of course, and possibly
excepting some special niceties, the practice are of universal
application.
The wine industry is somewhat less than 200 years old in
the United States. It has successfully taken root in some of the
Eastern and Middle States and principally in California and
Texas. The first successful cultivation of American wine grape-
vines was carried out in California in 1770 at the San Diego
Mission of the Franciscan Padres. They used a Spanish vine
which had been successfully transplanted in Mexico. The first
real attempt to cultivate the grapevine on a commercial scale in
California was probably around 1861 when the state government
backed Colonel Haraszthy in a trip to the principal grape grow-
ing districts of the world. He visited Europe, Asia Minor,
Persia and Egypt and returned with 200,000 cuttings of vines
which he believed likely to grow in California. A nursery was
established at Sonoma and a study was made of the possibilities
of the transplanted vines. Subsequently, the first State Board
of Viticultural Commission, the United States Department of
Agriculture and University of California, imported other clip-
pings which were also tested. As a result vines were soon dis-
tributed and planted in all suitable localities of the state. Ex-
perienced European grape-growers and wine-makers were then
induced to settle in the state and in course of time the well-known
Californian industry was established successfully. As a result of
this farseeing and well organized undertaking California, today,
is able to imitate the wines of practically any district of the world.
Many attempts were also made in Eastern states to establish
vineyards and to found an Eastern wine industry, procedure be-
ing much along the same lines as those tried successfully in Cali-
fornia. Unfortunately, European grapes will not flourish in
these sections of the United States and all such attempts ended
in disaster. About the middle of the last century Nicholas Long-
worth, Sr., experimented with the native Catawba grape in Ohio
38 RAW MATERIALS
and was so successful that the Ohio River was often referred to
as the "Rhineland of America." This undertaking also came to
a disastrous ending when disease attacked the vines. However,
fresh plantings of American Vine Roots and Hybrids along the
shores of Lake Erie and in Steuben County, New York, and
parts of New Jersey have been more successful.
Geographical Considerations. The choice of a site for
grape production, as indicated previously, depends very largely
on the nature of the soil and the climate. The following tabu-
lation of grapes successfully grown in the United States will illus-
trate this statement:
TABLE VII. AMERICAN GRAPE VARIETIES
Lake Shore District of Ohio
Catawba, Delaware, Concord, Norton
Steuben County, New York
Arranged in the order of merit:
Delaware, lona, Diana, Catawba, Concord, Isabellas, Norton
Southern Texas
Devereux (Black July), Mustang, Herbemont, Lenoir (known as
Burgundy in eastern Texas and Black Spanish in western Texas).
California
Fresno County
Zinfandel, Malvoisie and Fahirzozos.
Zinfandel is considered best grape; color, excellent; flavor and acid,
splendid.
Sonoma Valley
Mission, Riesling, Gutedel (Chasselais), Muscatel, Burger, Zin-
fandel.
The Mission grape has spread over the whole state and is much
used in the production of Hock, Claret, Port and Angelica.
Napa County
Riesling, White, Pineau and Chasselais for dry white wines.
Black Burgundy, Zinfandel and Charboneau for Claret. The first
makes a dark, full bodied and richly flavored wine. The second
has a fine raspberry flavor but an excess of acid and is a little light
in body and color.
Black Malvoisie is tbe best Port wine grape.
WINE MATERIALS 39
Bioletti (California Agr. Exp. Sta. Bull. 193. "The Best
Wine Grapes of California"} has summarized the geographical
and climatic factors which must he borne in mind. While his
statement is with particular reference to California, the principles
which he enunciates are of general validity. He says:
"For the good of the industry at large it is desirable that varieties
should be planted which will produce as large a crop as is compatible with
such quality as will maintain and extend the markets for our wine. These
markets are varied in character. For some, cheapness is the essential
factor; for others, quality. Cheap wines can be produced with profit only
from heavy-bearing varieties grown in rich soil ; wines of the highest qual-
ity only from fine varieties grown on hillsides or other locations where the
crops are necessarily less. It is therefore unwise to plant poor-bearing
varieties in the rich valleys where no variety can produce a fine wine. It
is equally unwise to plant common varieties on the hill slopes of the Coast
Ranges where no variety will produce heavy crops. The vineyards of the
San Joaquin, Sacramento, and other valleys can not compete with the
vineyards of the Coast Ranges in quality, and the latter can not compete
with the former in cheapness.
Each region has its own special advantages which, if properly used,
will make grape-growing profitable in all, and instead of competing each
will be a help to the other. The danger to be feared by the grape-growers
of the Coast Ranges from the production of dry wine in the interior is not
competition, but lies in the bad reputation given to California wines by
the production of spoiled and inferior wines. If the cheap wines of the
valleys are uniformly good and sound the market for the high-priced fine
wines of the hills will increase, and large quantities of the Coast Range
wines will be used for blending with the valley wines to give them the
acidity, flavor and freshness which they lack.
In order to obtain these results it is necessary that varieties suited to
each region and to the kind of wine should be planted. No variety which
is not capable of yielding from 5 to 8 tons per acre in the rich valley soils
or from i l /2 to 3 tons on the hill slopes should be considered. On the
other hand, no variety which will not give a clean-tasting, agreeable wine
in the valley or a wine of high quality on the hills should be planted,
however heavily it may bear. To plant heavy-bearing inferior varieties
such as Burger, Feher Szagos, Charbono, or Mataro on the hills of Napa
or Santa Cruz is to throw away the chief advantage of the location. The
same is true of planting poor-bearing varieties such as Verdelho, Chardo-
nay, Pinot, or Cabernet Sauvignon in the plains of the San Toaquin.
RAW MATERIALS
With these considerations in view, the following suggestions are made
for planting in the chief regions of California:
WINE GRAPES RECOMMENDED FOR CALIFORNIA
For Coast Counties
Red Wine Grapes
1. Petite Si rah
2. Cabernet Sauvignon
3. Beclan
4. Tannat
5. Serine
6. Mondeuse
7. Blue Portuguese
8. Verdot
White Wine Grapes
1 . Semillon
2. Colombar (Sauvignon vert)
3. Sauvignon blanc
4. Franken Riesling
5. Johannisberger
6. Tsaminer
7. Peverella
For Interior Valleys
Red Grapes
1. Valdepenas
2. St. Macaire
3. Lagrain
4. Gros Mansene
5. Barbera
6. Refosco
7. Pagadebito
White Grapes
1. Burger
2. West's White Prolific
3. Vernaccia Sarda
4. Marsanne
5. Folle blanche
For Sweet Wines
Red Grapes
1. Grenache
2. Alicante Bouschet
3. Tinta Madeira
4. California Black Malvoisie
5. Monica
6. Mission
7. Mourastel
8. Tinta Amarelia
White Grapes
1. Palomino
2. Beba
3. Boal
4. Perruno
5. Mantuo
6. Mourisco branco
7. Pedro Ximenez
Finally, a few suggestions as to what "not to do."
Don't plant Mataro, Feher Szagos, Charbono, Lenoir, or any variety
which makes a poor wine everywhere.
Don't plant Burger, Green Hungarian, Mourastel, Grenache, or any
common heavy-bearing varieties on the hill slopes of the Coast Ranges.
LIQUEURS AND CORDIALS 41
Vineyards in such situations must produce fine wines, or they will not be
profitable.
Don't plant Chardonay, Pinot, Cabernet Suavignon, Malbee, or any
light-bearing varieties in rich valley soils. No variety will make fine, high-
priced wine in such situations, and heavy bearers are essential to the pro-
duction of cheap wines.
Don't plant Zinfandel, Alicante Bouschet, or any of the varieties which
have already been planted in large quantities, unless one is sure that the
conditions of his soil and locality are peculiarly favorable to these varieties
and will allow him to compete successfully."
Liqueurs and Cordials. The raw materials for the manufac-
ture of liqueurs and cordials are necessarily classified in a different
manner from those used in the distilled spirit or wine industries.
In general they may be divided into three broad groups with sub-
divisions as indicated:
A. Flavoring Agents
1. Herbs, spices, seeds, roots, and fruits.
2. Aromatic spirits and tinctures.
3. Aromatic waters.
4. Essential Oils.
B. Coloring Agents
1. Vegetable Coloring Matters.
2. "Aniline" dyes. (Synthetic dyestuffs.)
C. Bulk Ingredients
1. Sugar and glucose.
2. Brandies or rectified spirits.
3. Water.
The number of materials included in Group Ai above is
very large; among others the following find principal use:
HERBS, SEEDS, ROOTS, SPICES, BARKS, FRUITS, ETC.
Chinese aniseed Cocoa Caraque
Bitter almonds Cocoa Maragnan
Green an is Mace
Coriander Vanilla
Fennel Figs
Angelica root Cumin
-Angelica seed Calamus, aromatic
Lemon peel Peel of Dutch Curacao
RAW MATERIALS
Orange peel
Anis de Tours
Anis d'Albi
Ceylon cinnamon
Orris
Cloves
Marjoram
Sweet almonds
Nutmeg
Sassafras
Muskseed
Apricot stones
Cherry stones
Dried peach leaves
Dried peaches
Myrrh
Quince juice
Strawberries
Nuts
Pineapple
Angostura bark
In Group A 2 will be found:
Aloes
Saffron
Curacao reeds
Wormwood
Hyssop Flowers
Lemon balm
Cherries
Alpine mugwort
Arnica Flowers
Peppermint
Balsamite
Thyme
Tonka beans
Black currants
Black currant leaves
Quinces
Red Sandalwood
Liquorice wood
Ginger root
Galanga root
AROMATIC SPIRITS
Anis
Angelica root
Angelica seeds
Curacao
Peppermint
Apricot
Lemons
Coriander
Amberseed
Dill
Caraway
Daucus
Fennel
Strawberries
Group A 3 includes:
Orange Flower
Peppermint
Rose
Celery
Aloes
Myrrh
Saffron
Chinese cinnamon
Cloves
Nutmeg
Orange Flowers
Bitter Almonds
Cardamom major
Cardamom minor
Oranges
Nuts
AROMATIC WATERS
Moka
Chinese aniseed
Clove
LIQUEURS AND CORDIALS 43
Group A4 includes the flavoring principles derived from
any of the raw materials listed under the heading of Group A2.
The term "essential oils'* is a generic commercial phrase used to
designate the volatile oils obtained by various processes such as
steam distillation, expression, maceration, enfleurage and solvent
extraction, from the specific plant or part of a plant which gives
them their name. The term is derived from the word "essence"
meaning that in these oils is contained the soul or strength of the
plant. In fact, in some countries, the single word is used instead
of the longer "essential oil." In the United States, however, the
usage is that the term "essence" or "spirits of" applies rather
to a solution in alcohol of the "essential oil." And a new phrase
"soluble essence" has been invented to describe essences which are
completely miscible with water or dilute alcohol without separa-
tion of the oil taking place.
The essential oils exist in all odorous vegetable tissues, some-
times pervading the plant, sometimes confined to a single part;
in some instances, contained in distinct cells, and partially retained
after desiccation, in others, formed upon the surface, as in many
flowers, and evaporating as soon as formed. Occasionally two
or more oils are found in different parts of the same plant. Thus,
the orange tree produces one oil in its leaves, another in its
flowers, and a third in the rind of its fruit.
The volatile oils are usually colorless when freshly distilled,
or at most yellowish, but some few are colored brown, red, green
or blue. There is reason, however, to believe that in all instances
the color depends on foreign matter dissolved in the oils. They
have strong odors, resembling that of the plants from which they
were procured, though generally less agreeable. Their taste is
hot and pungent, and, when they are diluted, is often gratefully
aromatic. The greater number are lighter than water, though
some are heavier; their specific gravity varies from 0.847 to I - I 7-
They vaporize at ordinary temperatures, diffusing their particular
odor and are completely volatilized by heat.
The following is a partial list of coloring agents used in the
production of liqueurs and cordials:
44 RAW MATERIALS
VEGETABLE COLORS
Caramel Indigo (Sulphonated)
Cherry Extract Orchil
Chlorophyll preparations Saffron
Cochineal Vanilla Extract
Cudbear
SYNTHETIC DYESTUFFS
In France the artificial coloring agents used are subject to less
limitation than in the United States, and since France is the
largest producer of cordials the following list is appended:
Rose Bengal Bleu de lumiere
Rouge de Bordeaux Bleu coupler
Fuchsine, acid Malachite green
Bleu de Lyon Violet de Paris (Gentian Violet 36)
It should be noted that not one of these dyes is included in
the United States list of colors certified for use in foods, which
only are permitted to be used in this country in interstate com-
merce and in many states in intrastate commerce. This list which
follows is varied enough to allow for the production of any
desired shade.
CERTIFIED FOOD COLORS
RED SHADES: GREEN SHADES:
80. Ponceau 3R. 666. Guinea Green B.
184. Amaranth. 670. Light Green SF Yellowish.
773. Erythrosine. Fast Green FCF.
Ponceau SX.
ORANGE SHADE: BLUE SHADES:
150. Orange I. 1180. Indigotine.
Brilliant Blue FCF.
YELLOW SHADES:
10. Naphthol Yellow S.
640. Tartrazine.
22. Yellow AB.
61. Yellow OB.
Sunset Yellow FCF.
LIQUEURS AND CORDIALS 45
The numbers preceding the names refer to the colors as listed in the
Colour Index published in 1924 by the Society of Dyers and Colourists of
England, which gives the composition of these dyes. Names not preceded
by numbers are not listed in the Colour Index.
No description is here necessary of the materials which we
have classified as group C above. A description of their specific
employment will be found in subsequent chapters devoted to
manufacturing operations. The same applies to a number of
minor ingredients or materials used for special purposes such as
souring, fining, preserving, sterilizing, etc.
CHAPTER V
YEASTS AND OTHER ORGANISMS
General Statement. In the preceding chapter on Fermenta-
tion it was stated that the production of alcohol is performed by
enzymes which act on the sugars present in the fermenting liquor.
It was also indicated previously that the enzymes which accom-
plish this transformation are representative of a very large group
of such materials which function in every chemical change in-
volved in the life process. The enzymes of value to the
fermentation industry are produced by living plants, yeasts, which
are allowed to grow in the liquor to be fermented and which,
as an incident of their own life process, achieve the desired pro-
duction of alcohol.
Yeasts belong to the second broad group of vegetable
growths : those which do not contain chlorophyll and are, there-
fore^ unable to manufacture their own food. This group is
distinguished from the first group of plants which can extract
inorganic materials from the soil and the air and from these
manufacture their own food. The ability to perform this function
is ascribed to the presence in the plant of a green coloring matter,
chlorophyll.
The group name of the non-chlorophyll bearing plants is
fungi. They are all dependent for their food supply upon the
materials built up by living plants of group one, or upon animal
matter. Among the fungi, which naturally vary in complexity
of structure, are a group of simply constructed plants having but
one cell and which are called yeasts. The cells vary in shape
and size, being round, oval or elongated, but of the order of
0.003 inches in diameter.
Each such cell consists of a transparent elastic sac or mem-
brane enclosing a more or less granular mass of jelly-like sub-
stance which is called protoplasm. The name was originated by
46
LIFE PROCESSES 47
Purkinje (ca. 1840) to apply to the formative material of young
animal embryos. Later, von Mohl (ca. 1846) used the term
to distinguish the substance of the cell body from that of the
nucleus which he called cytoplasm. In modern usage dating from
Strasburger (ca. 1882) the name protoplasm has been applied to
all of the essential living substance within the cell wall and means
the form of matter in or by which the phenomena of life are
manifested. Protoplasm can exist in many modifications varying
from its usual one of a thick, viscous, semi-fluid, colorless, trans-
lucent mass containing a high proportion of water and holding in
suspension fine granular material. Chemical examination of pro-
toplasm, necessarily after death, has shown that it is composed
largely of protein material. During its life, however, it appears
probable that the chemical composition is both more complex
and more unstable. For our purpose it is only necessary to state
that the protoplasm is that portion of the plant which is alive and
which carries on the vital processes of the plant.
Life Processes. All living organisms exemplify the cycle of
birth, growth, multiplication and death. Starting, for yeast, at
the stage of growth we see the process as follows: When the
yeast is supplied with an abundance of nutrient material, it grows
vigorously and the cellular protoplasm is homogeneous. As the
growth continues and the nutrient material becomes exhausted,
clear, apparently empty, spaces called vacuoles appear in the
protoplasm. Actually these spaces are filled with serum or sap.
At a little later stage, granules appear, some of which are fat
globules while others are more condensed portions of proto-
plasm. Finally, as the cell nears the end of its life, the proto-
plasm shrinks to a thin layer against the cell wall while the bal-
ance of the cell is occupied by a large vacuole. The nucleus of
the cell is rarely visible and does not, for this reason, enter into
our consideration.
While this growth of the single cell continues, multiplication
also takes place at a rapid rate. According as the life conditions
are favorable or not multiplication takes place in one of two
ways :
1. By budding or germination.
2. By endogenous division or ascospore formation.
48 YEASTS AND OTHER ORGANISMS
The first process occurs under favorable conditions when the
yeast is growing rapidly. It consists in a bulging of part of
the cell wall and the pressing of part of the cell contents into
the bulge which is formed. This is the bud. As the bud grows the
wall between it and the mother cell constricts and finally closes
and there are then two distinct cells. Whether the bud-cell stays
in connection with the mother cell depends somewhat on the
conditions of growth but more on the variety of yeast. With
some varieties the bud stays in connection with the mother cell
and itself multiplies through many generations so that long chains
or branching clusters are formed. In all cases the rapidity of
multiplication depends on the vigor of the yeast and the suitability
of the conditions under which it is growing.
In distinction to the method of reproduction just described,
when a vigorous yeast growth is placed into adverse conditions
it prepares to survive by a different mode. The protoplasm of
the cells becomes granular, then divides so as to form separate
masses. These round off and become invested with a wall so
that the original cell wall acts merely as a sac to contain the new
bodies. Because of this last fact the name ascospores is given
them, meaning spores formed within a sac. The conditions re-
quired to bring about ascospore formation are not completely
understood. Usually, however, a suitable temperature, plenty
of moisture and lack of nutrient material will cause young, vigor-
ously growing yeast cells to form from one to four ascospores
each. The spores have remarkable ability to survive under con-
ditions which would be fatal to ordinary cells; such as extremes
of temperature, lack of food, drying out, etc.
When at some future time the spores are placed into favor-
able conditions for growth they germinate and start a new series
of the ordinary type of yeast cells. In germinating they exert
a pressure against the wall of the mother cell which finally breaks
and permits the escape of the new cells. In some cases actual
dissolution of the cell occurs during germination.
.The changes described above are well illustrated in the ac-
companying figure, which shows stages in the life of a favorable
pure culture yeast and also some of the mixed forms.
CLASSIFICATION OF YEASTS
49
Classification of Yeasts. Although the structure of yeasts is
so exceedingly simple that it seems difficult for varieties to exist,
nevertheless there are many different kinds or species. The dis-
tinctions are partly morphological, i.e., in the physical form of
the cells, and partly chemical, i.e., in the enzymes elaborated by
the cells which, of course, means that the products resulting from
*&.
'0
FIG. 2. True Wine yeast.
i. Yeast cells in fermenting grape juice (mixed forms).
2. Saccharomyces ellipsoideus (spores).
3. Saccharomyces ellipsoideus (old).
4. Saccharomyces ellipsoideus (young).
the action of different yeasts on the same medium or substrate
will be different. When a pure yeast is used in fermentation, an
entirely different result is obtained than from the use of an im-
pure. The flavor is different, as also the odor, and with a pure
yeast the keeping properties are better. For the purposes of the
fermentation industry, yeasts are divisible into two groups:
50 YEASTS AND OTHER ORGANISMS
1. The wild yeasts those which occur in nature; floating in
the air, in the soil, and on^the skins of fruits.
2. The cultivated yeasts which have been selected from the
wild yeasts for their favorable action and are carefully guarded
in laboratory and factory to insure purity of strain.
There are two schools of thought in the fermentation indus-
try and especially among wine makers as to whether it is prefer-
able to use pure culture yeasts or to depend on wild yeasts. On
the one hand it is claimed that pure culture yeast will result in
a more accurately controlled fermentation, in a reduction in the
time and labor required for racking and aging, a cleaner taste
and flavor, and in the ability to select beforehand the flavor
desired.
On the other hand, it is claimed that these advantages are
offset by the necessity of sterilizing the must, pressed grapes and
juice. In practice, however, the benefits derived from the use
of pure culture yeast can often be had without resorting to the
costly operation of sterilization. The pure culture yeasts are
especially advantageous in the manufacture of white and sparkling
wines and in the refermentation of the latter. They are used ex-
tensively abroad for these purposes and have secured some recog-
nition and produced excellent results in some wineries in this
country.
In whiskey distilleries, pure culture yeasts have been used ex-
tensively in recent years. The types are selected for high alco-
hol yields and propagated by the Hansen single-cell method.
There can be no doubt at the present time but that pure culture
yeasts are an absolute necessity for the manufacture of distilled
spirits and very much preferable for the manufacture of wines.
The principal yeasts encountered in spirit and wine manufac-
ture are :
Saccharomyces cerevisiae. The ordinary yeast of the brewer and the
distiller. Two kinds are recognized: (a) top fermentation, and (b) bot-
tom fermentation.
Top yeast, as its name implies, is a type which rises in a frothy mass to
the top of the mash during fermentation. Bottom yeast sinks to the bot-
tom of the vat during fermentation. Higher temperatures favor the for-
MICRO-ORGANISMS FOUND ON GRAPES 51
mation of the former and lower temperatures favor the latter. Distillers'
yeast is a high attenuating top variety.
Saccharomyces ellipsoideus. This is the yeast which converts must, or
grape juice, into wine.
Saccharomyces pastorianus. This also occurs in wine making and when
present during brewing gives a bitter taste to the beer.
Saccharomyces mycoderma. This yeast is the cause of "mother 11 which
appears on the surface of wine or beer after exposure for some days to
the air.
Bakers use either compressed yeast (compressed cakes of
top yeast) or dried yeast (a mixture of yeast cells with starch).
The former has high fermenting capacity and gives uniform
results, but it will keep only a day or two; while the latter retains
its capacity to produce fermentation for a long period. Brewers*
yeast is not desirable for bread making because it is likely to give
a bitter flavor and its activity is slow in a dough mixture.
Pure Cultures. To determine the properties due to a par-
ticular yeast, it must be separated from all other organisms with
which it is associated and when grown thus, free from all con-
tamination, it is then known as a "pure culture. " A commercially
pure yeast is different, as this simply means "free from added
non-yeast matter." This is the condition of most compressed
yeasts as found on the market; they are commercially, but not
bacteriologically, pure, since they have numbers of bacteria and
molds associated usually with more than one yeast variety.
Micro-Organisms Found on Grapes. The surfaces of
grapes in the vineyard will hold any or all of the bacteria and
fungi usually carried in the air and by insects. Many of these,
especially the bacteria, cannot grow in grape juice on account of
its acidity. These, of course, have a negligible effect on the wine.
Others, such as most yeasts and molds and a few varieties of
bacteria find grape juice to be a favorable medium for their de-
velopment. Wine is a somewhat less suitable medium than
unfermented grape juice (must], owing to its alcohol content,
but still, a large number of forms are capable of growing in the
wine. As the wine ages, the less suitable it becomes for the
growth of micro-organisms, but it is never quite immune.
Among the great variety of organisms the only ones desired
52 YEASTS AND OTHER ORGANISMS
are the wine yeasts. Many different types of wine yeast have
been isolated and studied. It has been demonstrated that not
only do slight morphological differences exist, but also that they
vary in the flavor and quality of wine produced and also in the
speed and completeness with which they split sugar and consume
acids. The true yeasts occur much less abundantly on grapes than
the molds. Until the grapes are ripe they are practically absent,
as first shown by Pasteur. Later, they gradually increase in
number; on very ripe grapes being often abundant. In all cases
and at all seasons, however, their numbers are much inferior to
those of the molds and pseudo-yeasts. The cause of this seems
to be that, in the vineyard, the common molds find conditions
favorable to their development at nearly all seasons of the year,
but yeasts only during the vintage season.
Investigations of Hansen, Wortmann and others show that
yeasts exist in the soil of the vineyard at all times, but in widely
varying amounts. For a month or two following the vintage, a
particle of soil added to nutritive solution contains so much yeast
that it acts like a leaven. For the next few months the amount
of yeast present decreases until a little before the vintage, when
the soil must be carefully examined to find any yeast at all. As
soon as the grapes are ripe, however, any rupture of the skin of
the fruit will offer a favorable nidus for the development and
increase of any yeast cells which reach it. Where these first
cells come from has not been determined, but as there are still a
few yeast cells in the soil, they may be brought by the wind, or
bees and wasps may carry them from other fruits or from their
hives and nests.
The increase of the amount of yeast present on the ripe
grapes is often very rapid and seems to have (according to
Wortmann) a direct relation to the abundance of wasps. These
insects passing from vine to vine, crawling over the bunches to
feed on the juice of ruptured berries, soon inoculate all exposed
juice and pulp. New yeast colonies are thus produced and the
resulting yeast cells quickly disseminated over the skins and other
surfaces visited.
The more unsound or broken grapes present, the more honey-
PSEUDO- YEASTS 53
de\v or dust adhering to the skins, the larger the amount of
yeast will be. The same is true, however, also of molds and
other organisms.
True Wine Yeasts Saccharomyces ellipsoideus. In the
older wine-making districts, much of the yeast present on the
grapes consists of the true wine yeast, S. ellipsoideus. The race
or variety of this yeast differs, however, in different districts.
Usually several varieties occur in each district. The idea preva-
lent at one time, that each variety of grape has its own variety
of yeast seems to have been disproved, though there seems to be
some basis for the idea that grapes differing very much in com-
position, varying in acidity and tannin contents, may vary also in
the kind of yeast present. Several varieties of ellipsoideus may
occur on the same grapes. In new grape-growing districts, where
wine has never been made, ellipsoideus may be completely absent.
Besides the true wine yeast, other yeasts usually occur. The
commonest forms are cylindrical cells grouped as S. pasteurianus.
These forms are particularly abundant in the newer districts,
where they may take a notable part in the fermentation. Their
presence in large numbers is always undesirable, and results in
inferior wine. Many other yeasts may occur occasionally, and
are all more or less harmful. Some have been noted as produc-
ing sliminess in the wine. Many of these yeasts produce little or
no alcohol and will grow only in the presence of oxygen.
Pseudo-yeasts. Yeast-like organisms producing no endo-
spores always occur on grapes. Their annual life cycle and their
distribution are similar to those of the true yeast but some of them
are much more abundant than the latter. They live at the
expense of the food materials of the must and, when allowed to
develop, cause cloudiness and various defects in the wine.
The most important and abundant is the apiculate yeast, S.
apiculatus (according to Lindner this is a true yeast producing
endospores). The cells of this organism are much smaller than
those of S. ellipsoideus and very distinct in form. In pure cul-
tures these cells show various forms, ranging from ellipsoidal
to pear-shaped (apiculate at one end) and lemon-shaped (apicu-
late at both ends). These forms represent simple stages of de-
54
YEASTS AND OTHER ORGANISMS
velopment. The apiculations are the first stage in the formation
of daughter cells; the ellipsoidal cells, the newly separated daugh-
ter cells, which, later, produce apiculations and new cells in turn.
Many varieties of this yeast occur, similar in degree to those
of S. ellipsoideus. They are widely distributed in nature, occur-
ring on most fruits, and are particularly abundant on acid fruits
such as grapes. Apiculate yeast appears on the partially ripe
grapes before the true wine yeast and even on ripe grapes is more
abundant than the latter. The rate of multiplication of this yeast
FIG. 3. Yeasts and injurious pseudo-yeasts.
1. Torulae and pseudo-yeasts.
2. Torulae and pseudo-yeasts.
3. Saccharomyces apiculatus.
4. Saccharomyces pasteurianus.
5. Mycoderma vini (2 forms).
6. Dematium pullulans.
is very rapid under favoring conditions and much exceeds that
of wine yeast. The first part of the fermentation, especially at
the beginning of the vintage and with acid grapes, is, therefore,
often almost entirely the work of the apiculate yeast.
The amount of alcohol produced by this yeast is about 4 per
cent, varying with the variety from 2 to 6 per cent. When the
fermentation has produced this amount of alcohol, the activity of
the yeast slackens and finally stops, allowing the more resistant
ellipsoideus to multiply and finish the destruction of the sugar.
PSEUDO- YEASTS 55
The growth of the apiculatus, however, has a deterring effect on
that of the true yeast so that where much of the former has been
present, during the first stages of the fermentation, the latter
often fails to eliminate all the sugar during the final stages.
Wines in which the apiculate yeast has had a large part in
the fermentation are apt to retain some unfermented sugar and
are very liable to the attacks of disease organisms. Their taste
and color are defective, often suggestive of cider, and they are
difficult to clear. This yeast attacks the fixed acids of the must,
the amount of which is therefore diminished in the wine while,
on the other hand, the volatile acids are increased.
Many other yeast-like organisms may occur on grapes; but,
under ordinary conditions, fail to develop sufficiently in competi-
tion with apiculatus to have any appreciable effect on the wine.
Most of them are small round cells, classed usually as Torulae.
They destroy the sugar but produce little or no alcohol.
A group of similar forms, known collectively as Mycoderma
vini, occurs constantly on the grapes but, all being strongly
aerobic, they do not develop in the fermenting vat. Under
favoring conditions, however, they may be harmful to the fer-
mented wine.
Bacteria of many kinds occur on grapes as on all surfaces
exposed to the air. Most of these are unable to develop in solu-
tions as acid as grape juice or wine. Of the acid-resisting kinds,
a number may cause serious defects and even completely destroy
the wine. These, the u disease bacteria" of wine are mostly
anaerobic and can develop only after the grapes are crushed and
the oxygen of the must exhausted by other organisms. Practically
all grape-must contains some of these bacteria, which, unless the
work of the wine-maker is properly done, will seriously interfere
with the work of the yeast, and may finally spoil the wine. The
only bacteria which may injure the grapes before crushing are
the aerobic, vinegar bacteria, which may develop on injured or
carelessly handled grapes sufficiently to interfere with fermenta-
tion and seriously impair the quality of the wine.
Among the organisms which can infect wine and cause so-
called "diseases" are the following:
56 YEASTS AND OTHER ORGANISMS
Molds. The spores of the common saprophytic molds, Penicillium,
Aspergillus, Mucor, Dematium, are always present on the grapes, boxes,
and crushers, as on all surfaces exposed to dust laden air, and most of them
find in grape must, excellent conditions for development. Botrytis cinerea,
a facultative parasite of the leaves and fruit of the vine, is also nearly
constantly present in larger or smaller quantities. All of these molds are
harmful, in varying degrees, to the grapes and the wine. Some of them,
such as Penicillium, may give a disagreeable moldy taste to the wine, suffi-
cient to spoil its commercial value. Others, such as Mucor and Asper-
gtlius may affect the taste of the wine but slightly and injure it only by
destroying some of the sugar and thereby diminishing the final alcohol
content. Dematium pullulans may produce a slimy condition in weak
white musts, and most of them injure the brightness and flavor to some
extent and often render the wine more susceptible to the attacks of more
destructive forms of micro-organisms.
On sound, ripe grapes, these molds occur in relatively small number,
and, being in the spore or dormant condition, they are unable to develop
sufficiently to injure the wine under the conditions of proper wine-making.
On grapes which are injured by diseases, insects or rain, they may de-
velop in sufficient quantities to spoil the crop before it is gathered. On
sound grapes which are gathered and handled carelessly, they may develop
sufficiently before fermentation to injure or spoil the wine.
The molds are recognized by their white or grayish cobwebby growth
over the surface of the fruit. This consists of fine branching and inter-
lacing filaments known as mycelium. This is the vegetative stage of the
fungus and the active part in the destruction of the material attacked.
When mature, it produces spores which differ for each mold in form, size
and color. The spores are the chief means of multiplication and distri-
bution. They are minute, single celled bodies which are easily distributed
as dust through the air, and are capable, after remaining dormant for a
longer or shorter period, of germinating, under favorable conditions and
giving rise to a new growth of mycelium.
The commonest molds on grapes in California are the Blue Mold, the
Black Mold and the Gray Mold. Usually only one of these occurs plenti-
fully at the same time. Which this one will be depends principally upon
the temperature and humidity. In the hotter regions the Black Mold is
most common during the earlier part of the vintage, later the Blue Mold
takes its place. In the cooler regions only Gray and Blue Molds occur
commonly.
Blue Mold (Penicillium glaucum). This is the common mold which
attacks all kinds of fruit and foods kept for a length of time in a damp
place. It is distinguished by the greenish or bluish color of its spores
which cover the grapes attacked, and by its strong disagreeable moldy
smell. It sometimes attacks late grapes in the vineyard after autumn rains
PSEUDO-YEASTS 57
have caused some of them to split. Grapes lying on the ground are espe-
cially liable to attack. The principal damage of this mold occurs usually,
after the grapes are gathered, while they lie in boxes or other containers.
It will grow on almost any organic matter if supplied with sufficient
moisture and at almost any ordinary temperature. It is almost the sole
cause of all moldiness in boxes, hoses, and casks, and the most troublesome
of all the molds with which the wine-maker has to deal.
The conditions most favorable to its development are an atmosphere
saturated with moisture and the presence of oxygen.
Black Mold (Aspergillus niger). This is very common in the hotter
and irrigated parts of California. It annually destroys many tons of grapes
before they are gathered. It attacks the grapes just as they ripen and is
distinguished by the black color of its spores, which sometimes fill the air
with a black cloud at the wineries where the grapes are being crushed. It
is especially harmful to varieties which have compact bunches and thin
skins, such as Zinfandel. Its effect on the wine has not been well studied
but it is much less harmful than Green Mold. Large quantities of grapes
badly attacked are made every year into merchantable wine. The main
damage done is in the destruction of crop and it is therefore a greater
enemy to the grape-grower than to the wine-maker.
Gray Mold (Botrytis cinerea). This fungus in certain parts of Europe
is a harmful parasite of the vine, injuring seriously leaves, shoots and
growing fruit. The only injury of this kind noted in California is in the
"callousing" beds of bench grafts.
As a saprophyte it may attack the ripe grapes in much the same manner
as the Black Mold. It occurs apparently all over California but seldom
does much damage. It attacks principally second crop and late table
grapes.
Under certain circumstances this fungus may have a beneficial action.
When the conditions of temperature and moisture are favorable, it will
attack the skin of the grape, facilitating evaporation of water from the
pulp. This results in a concentration of the juice. The mycelial threads
of the fungus then penetrate the pulp, consuming both sugar and acid but
principally the latter. The net result is a relative increase in the per-
centage of sugar and a decrease in that of acid. This, where grapes ripen
with difficulty, is an advantage, as no moldy flavor is produced. Two
harmful effects, however, follow: First, the growth of the mold results
in the destruction of a certain amount of material and a consequent loss of
quantity. This is, in certain circumstances, more than counterbalanced by
an increase in quality, as is the case with the finest wines of the Rhine and
Sauternes. For this reason, the fungus is called in those regions the "Noble
Mold." Second, an oxydase is produced which tends to destroy the color
brightness and flavor of the vine. This may be counteracted by the judi-
cious use of sulfurous acid.
YEASTS AND OTHER ORGANISMS
FIG. 4. Wine grape molds.
1. Black mold (Aspergillus niger). (After Duclaux.)
a. Fruiting hyphae.
b. Sporecarp showing formation of spores.
c. Spores.
2. Gray mold (Botrytis cinerea). (After Ravaz.)
3. Blue mold (Penicillium glaucum). (From skin of moldy grape.)
a. Mycelium.
b. Fruiting hypha.
c. Chains of spores.
d. Spores.
CONTROL OF YEASTS
59
This mold is not of great importance in California as its beneficial
effects are not needed and there is seldom enough to do much harm.
The special organisms which cause diseases in wine include:
Anaerobic organisms such as Dematlum pullulans induce
slimy fermentation which results in "ropiness." These bacteria
attack the sugar, but not glycerin nor alcohol and produce man-
mite, carbon dioxide, lactic and acetic acids and alcohol. Their
FIG. 5. Disease Bacteria of wine.
1. Bacteria of mannitic wine.
2. Bacteria of bitter wine (butyric).
3. Bacteria of vinegar (b. aceticum).
4. Bacteria of lactic acid, young.
(a) Cell of wine yeast.
5. Bacteria of lactic acid, old.
6. Bacteria of slimy wine.
growth is entirely prevented by the presence of alcohol above thir-
teen per cent, free tartaric, tannic or small amounts of sulphurous
acid. The infection is ordinarily not very serious and disappears
under ordinary cellar treatment.
Botrytis and Penicilliiim which when present cause oxidation
of the tannin causing a bitter taste. This is more common in
red wines.
Acetic acid bacteria which cause the further oxidation of al-
cohol to acetic acid and result in a "pricking" taste. This taste
60 YEASTS AND OTHER ORGANISMS
is noticeable even when there is only 0.1-0.15% of acetic acid. A
dry wine becomes practically undrinkable at 0.25% of acetic acid.
Saccharomyces apiculatus will cause some production of alco-
hol but affects the flavor adversely.
Mycoderma vini attack the alcohol changing it to carbon
dioxide and water and hence weaken the wine directly as well as
rendering it more susceptible to infection by other disease organ-
isms. It is sometimes the cause of film.
Control of Yeasts. Control of the growth of these organ-
isms and even to some extent selection of the variety which shall
grow is largely possible by a consideration of the factors affecting
their vigor.
Nutrition. The preferred food of the yeasts is the sweet
juice of more or less acid fruits. Most of them are active agents
of alcoholic fermentation breaking up the sugar into alcohol and
carbonic acid gas. Wine yeast may carry on the fermentation
until the liquid contains 15 per cent or slightly more of alcohol.
Other yeasts, such as ordinary beer yeast cease their activity when
the alcoholic strength of the liquid reaches 8 to 10 per cent, while
some wild yeasts are restrained by 2 to 3 per cent.
Delation to Oxygen. They are aerobic, that is, they require
the oxygen of the air for their development. Most of them are,
however, capable of living and multiplying for a limited time in
the anaerobic condition, that is, in the absence of atmospheric oxy-
gen. It is in the latter condition that they exhibit their greatest
power of alcoholic fermentation. They multiply most rapidly
and attain their greatest vigor in the presence of a full supply of
air. In fermentation, therefore, it is necessary, first, to promote
their multiplication and vigor by growing in a nutritive solution
containing a full supply of oxygen and, then, to make use of
their numbers and vigor to produce alcoholic fermentation in a
saccharine solution containing a limited supply of oxygen. These
conditions are brought about automatically in the usual methods
of wine-making. The stemming and crushing of the grapes thor-
oughly aerates the must. The yeast multiplies vigorously in this
aerated nutritive solution until it has consumed most of the dis-
solved oxygen. It then exercises its fermentative power to break
CONTROL OF YEASTS 61
up the sugar, with the production of alcohol. With many musts
it is able in this way to completely destroy all the sugar without
further oxygen. In other musts, especially those containing a
high percentage of sugar, the yeast becomes debilitated before
the fermentation is complete. In such cases it is generally neces-
sary to reinvigorate it by pumping over the wine or by some other
method of aeration before it can complete its work.
Relation to Temperature. Yeast cells can not be killed or
appreciably injured by any low temperature. They do not be-
come active, however, until the temperature exceeds 32 F. Wine
yeast shows scarcely any activity below 50 F., and multiplies
very slowly below 60 F. Above this temperature the activity
of the yeast gradually increases. Between 70 F. and 80 F.
it is very active and it attains its maximum degree of activity
between 90 F. and 93 F. Above 93 F. it is weakened, and
between 95 F. and 100 F. its activity ceases. At still higher
temperatures the yeast cell dies. The exact death point depends
on the condition of the yeast, the nature of the solution and the
time of exposure. In must and wine a temperature of 140 F.
to 145 F. continued for one minute is usually enough to destroy
the yeast.
The best temperature in wine-making will depend on the kind
of wine to be made and will lie between 70 F. and 90 F.
Relation to Adds. The natural acids of the grapes, in the
amounts in which they occur in must, have little direct effect on
wine yeast. Indirectly they may be favorable by discouraging the
growth of competing organisms more sensitive to acidity. Acetic
acid has a strong retarding influence which commences at about
0.2 per cent and increases with larger amounts until at 0.5 per
cent to i.o per cent, according to the variety of the yeast, all
activity ceases.
Relation to Sulfurous Acid. Sulfurous acid is an antiseptic,
mild or strong, according to the quantities used. The fumes of
burning sulfur are used in various ways and for various purposes
in wine-making. The active principle of these fumes is sulfurous
acid gas of which the chemical formula SO 2 shows that it is
composed of one. atom of sulfur combined with two atoms of
62 YEASTS AND OTHER ORGANISMS
oxygen. As sulfur has just twice the atomic weight of oxygen
this means that one part by weight of sulfur combines with one
part by weight of oxygen to produce two parts by weight of
sulfurous acid gas. This combination takes place when sulfur
is burned in free contact with air. The same substance can be
obtained from certain salts, one of which is most suitable for use
in wine-making. This is a potash salt known as potassium meta-
bisulfite. This salt is composed of nearly equal weights of potash
and sulfurous acid. In contact with the acids of the must, the
sulfurous acid is set free and the potash combines with the tar-
taric acid of the must to form bi-tartrate of potash, some of
which is already present as a natural constituent of the must.
Bacteria of all kinds arc much more sensitive to the effects
of sulfurous acid than are yeasts. If used, therefore, in properly
regulated amounts it can be made a very efficient means of pre-
venting bacterial action and thus indirectly of aiding the work of
the yeast. It has also the very valuable property of preventing
the injurious action of the oxydase produced by Botrytis and
other molds. Finally, it is necessary in most cases to prevent
the too rapid or overoxidation of the wine during aging.
CHAPTER VI
PRODUCTION OF YEAST
Commercial Yeast. The application of the principles just
developed is well illustrated in the manufacture of yeast for gen-
eral use. The same niceties observed in this process must also
be followed in the production of so-called "starters" for the fer-
mentation of whiskey mashes or of wine must. Figure 6 is the
flow sheet of such a process. The exact proportions of the vari-
ous grains used are naturally varied according to the secret
formula of the manufacturer.
It will be noted that the steps on this flow sheet may be
divided by two horizontal lines into three broad divisions:
1. The first set of mechanical operations has for its object
the conditioning of the raw materials for the next set. It in-
cludes very thorough cleaning and purification of all the materials,
grinding the cereals to make them more reactive and steeping
them in water to further ease the dissolution of the nutritive
ingredients.
2. The next set of biochemical and chemical operations in-
cludes bringing the food for the yeast cells into the most readily
assimilable form and then growing the yeast in the medium so
produced under conditions which will result in the most vigorous
and prolific production of yeast.
3. In the final set of mechanical operations the yeast cells
are separated from the fermented liquor under the optimum con-
ditions to ensure their survival and prepared for marketing. The
actual operations involved in the process are somewhat as follows :
The cleaned, ground and steeped grains are cooked to pastify
the starch. Usually the corn is cooked first at the highest tem-
perature, then the rye is added and when the mash has cooled to
the proper temperature for the most effective action of diastase
(ca. 55 C, 130 F.) the malt is added.
63
PRODUCTION OF YEAST
[Barley Malt[ [ Rye [ | Corn | | Water | [ Sprouts [
Cleaner] [Cleaner| [Cleaner) I Filter \ |Cleaner|
i ' t
Mill | I Mill | | Mill
Fermenter
where
yeast
grows
Yeast Separators
~*f3) Separated
Mixing Machine
Cars to Agencies
Small
Lactic Acid
Mash
Shipping
Boxes
| Refrigerator
FIG. 6.
DISTILLERS' YEAST 65
When the diastase of the malt has had time to act the mash
is inoculated with a smaller special mash of rye and malt in which
a pure culture of lactic acid bacteria (Bacillus delbruckn} is
growing. The mash is now incubated for about sixteen hours at
the proper temperature (ca. 50 C., 122 F.). During this time
the proteins of the grains are partially hydrolyzed and some
lactic acid is formed. The liquor now contains largely sugars,
resulting from the action of malt diastase on the starch, lactic
acid, amino acids, and other hydrolysis products of the pro-
teins, all in a highly assimilable form for the yeasts, and the cellu-
lose residues from the cereals.
This sour mash is filtered and the filtrate, now called "wort,"
is heated (Pasteurized) to kill off the lactic acid bacteria and
any undesirable organisms. After cooling the wort is run into
fermentation tanks and inoculated with a pure yeast culture of
sufficient size. The wort is then aerated by passing in com-
pressed air either through bottom or side inlets. The oxygen of
the air bubbling through the wort stimulates the growth and
reproduction of the yeast cells.
When the growth of yeast has reached the desired extent, the
cells are separated from the fermenting wort in the third set of
operations. The ordinary equipment for this purpose is identical
in action with the familiar centrifugal cream separator. The
heavy cream of separated yeast is cooled, further water is re-
moved by means of a filter press. The press cake is churned,
squeezed in hydraulic presses, packed, and stored in a refriger-
ator.
Distillers' Yeast. Each manufacturer of distilled spirit pre-
pares the yeast for carrying on the production of alcohol in a
manner generally similar to that just described. The start is
usually made by reserving a portion from each completed fer-
mentation. The yeast in this reserved portion is propagated in
a small special mash made often from equal amounts of barley
malt and rye. In other distilleries only malt, either rye or barley,
is used; or possibly a mixture of one of these malts with a ground,
unmalted cereal such as wheat, barley or rye. In any case, the
object is to produce yeast cells which are young, vigorous and
66
PRODUCTION OF YEAST
so active that they will rapidly reproduce and will have a high
sugar splitting or fermentive capacity, to the end that the highest
possible yield of alcohol will result. A flow sheet of this process
is shown in Figure 7. It will be noted that it corresponds quite
closely to the main steps in the manufacture of ordinary yeast.
The ground rye is first scalded with water of about 170 F.
temperature. Then it is stirred, the ground malt added and the
whole mash kept for about two hours at a temperature of ap-
proximately 150 F. Its sugar content should be about 22 to
25 per cent as indicated on the Balling hydrometer.
Hot
Water
Ground
Rye
Barley
Malt
170F
Yeast reserved from
a previous fermentation
Mashing
150F and 22-25% Balling
Cooling
Souring
120F
Heating
170F
Cooling
Fermentation
80F
To main mash at 7 to 8% Balling
FIG. 7.
The mash is now cooled and soured. Sometimes a pure cul-
ture of lactic acid bacteria is added to speed up the souring
process. Cooling reduced the temperature of the mash about
thirty degrees, or to 120 F. When no lactic acid bacteria are
added it is kept at this temperature for about forty-eight hours
and souring is usually completed by that time. The addition of
bacteria reduces the time for souring to about eighteen hours, or
a little longer.
The souring process not only helps in the development of a
nutritive medium for the yeast but also the lactic acid formed
WINE STARTERS 67
prevents, or retards, the development of unfavorable micro-
organisms during fermentation, notably acetic acid bacteria.
As in commercial yeast manufacture, the lactic acid bacteria
are killed by heating the mash again; this time to 170 F. After
holding it at this point for about twenty minutes the temperature
is brought down to about 85 F. and the seed yeast is added.
Fermentation commences and the temperature is gradually low-
ered about five degrees. When the sugar content of the mash has
dropped to about 8 per cent Balling it is added to the main mash
where it represents about 5 per cent of the total volume.
Heating and cooling in all cases is obtained by the use of coils
for the circulation of hot or cold water in the tanks.
Wine Starters. Grapes ordinarily will produce a must which
contains sufficient yeast to carry on the fermentation. Unfortu-
nately, the must is also almost certain to contain many varieties
of unfavorable micro-organisms. Hence, especially in the manu-
facture of white wines some purging or sterilizing process is neces-
sary. The process ordinarily used is called defecation. This
consists of treating the must with sulfurous acid and is ordinarily
accomplished by pumping it into sulfurized casks (as described in
chapter on wine making). In from twelve to twenty-four hours,
the must is purged, and all its gross impurities, including micro-
organisms, dust and solid particles derived from the skins, stems,
pulp and leaves have settled to the bottom. It may be slightly
cloudy or nearly clear. It should then be drawn off into clean
casks and fermentation started. Sometimes it is sterilized by
Pasteurization following defecation, but this is not a very satis-
factory operation from the flavor standpoint; it is costly and is
generally dispensed with. In defecating must to eliminate un-
favorable micro-organisms the wine maker, unfortunately also
removes the true yeasts. The more perfect the process the more
necessary it is to add wine yeast. It is, therefore, necessary to
add a starter.
Natural Starters. One method of producing such a starter
is to gather a suitable quantity of the cleanest and soundest ripe
grapes in the vineyard, crush them carefully and allow them to
undergo spontaneous fermentation in a warm place. An addition
68 PRODUCTION OF YEAST
of a quarter to a third of an ounce of potassium meta-bisulfite per
hundred pounds of grapes is of great assistance in promoting
a good yeast fermentation in the starter. Perfectly ripe grapes
should be selected and the fermentation allowed to proceed until
at least 10 per cent of alcohol is produced. If imperfectly ripe
grapes are used or the starter used too soon, the principal yeast
present may be S. apiculatus. Towards the end of the fermenta-
tion S. ellipsoideus predominates. From one to three gallons of
this starter should be used for each hundred gallons of crushed
grapes or must to be fermented. Too much should not be used
in hot weather or with warm grapes, as it may become impossible
to control the temperature.
This starter is used only for the first vat or cask. Those
following are started from previous fermentations, care being
taken always to use the must only from a vat at the proper stage
of fermentation and to avoid all vats that show any defect.
Pure Yeast Starters. An improvement on a natural starter
of this kind is a pure culture of tested yeast. There are two
ways of using these yeasts. One is to obtain, from a pure yeast
laboratory, a separate starter for each fermenting vat or cask.
All the wine-maker has to do is to distribute this starter in the
grapes or must as they run into the vat. If the starter is used
when in full vigor this method is simple and effective. Unfortu-
nately, it is difficult to have it on hand in just the right condition
at the right moment. If the starter is too young, it will not
contain enough yeast cells; if too old, the cells will be inactive or
dead. The usual starter is in full vigor for only a few days
at the most. Recent improvements in the methods of preparing
pure yeast starters are said to overcome this difficulty and to
produce starters which maintain their full vigor for weeks or
months.
The other method is for the wine-maker to obtain a small cul-
ture of pure yeast from a reliable source and from this to make
his own starter.
To do this he prepares an innoculum of two or three gallons
of must defecated with sulfurous acid and sterilized by boiling.
This, on cooling, is placed in a large demijohn plugged with
WINE STARTERS 69
sterilized cotton and the pure culture of yeast added. The demi-
john must be placed in a warm place (70 to 80 F.) and
thoroughly shaken several times a day to aerate the must. In a
few days a vigorous fermentation occurs.
When the fermentation is at its height in the demijohn, which
will be when the must still contains 3 or 4 per cent of sugar, it is
ready to use to prepare a bulk starter. This is best prepared in a
small open vat or tub, varying in size according to the amount
of starter needed daily. Into this tub are poured twenty to fifty
gallons of well-defecated must extracted from clean, sound grapes.
It is not necessary to boil it, as the few micro-organisms it may
contain will be without effect in the presence of the vastly more
numerous yeast cells introduced from the pure culture in the
demijohn.
The whole of the pure culture is poured into the tub of must,
the temperature of which should be between 80 and 90 F. This
temperature is maintained either by warming the room or by
occasionally placing a large can full of boiling water in the tub.
This can should, of course, be tightly stoppered in order that
none of the water may get into the must. The must should be
well aerated several times a day to invigorate the yeast. This
is done by dipping out some of the must with a bucket or ladle
and pouring it back into the tub from a height of several feet or
by the use of compressed air. The tub should be covered with a
cloth to exclude dust, and everything with which the must comes
in contact should be thoroughly cleaned with boiling water.
In a day or two the must is in full fermentation and may be
used as a starter. From ten to thirty gallons of starter are used
for every thousand gallons of must or crushed grapes. The
cooler the grapes the more should be added. Too much added
to warm grapes may make the fermentation so rapid that it will
be difficult to control the temperature. Moldy or dirty grapes
require more than clean, because there are more injurious germs
to overcome.
Every twenty-four hours, nine tenths of the contents of the
starter tub can be used and immediately replaced with fresh
defecated must. The yeast in the remaining tenth is sufficient to
70 PRODUCTION OF YEAST
start a vigorous fermentation and multiplication of yeast. Two
things must be watched with special care if the starter is to main-
tain its vigor. The temperature must be kept above 80 F. and
thorough and frequent aeration must be given.
With care, a starter of this kind will remain sufficiently pure
to be used continuously throughout the vintage.
CHAPTER VII
MALT
In one very important respect the manufacture of spiritous
liquors from a grain base differs from that commencing with a
fruit juice base. This difference is that the fruit juices contain
preformed sugar directly available for fermentation while the
cereals contain starch and proteins in a relatively insoluble form.
It was stated in previous chapters that by suitable processes this
insoluble starch and proteins can be converted into soluble forms
which are then fermentable. The processes by which this con-
version is accomplished are the subject of this chapter.
There are two general means by which starch and proteins
are solubilized (hydrolyzed) for the purpose of fermentation.
These are by the action of suitable enzymes or by treatment with
acids. Of these the former is much more common in the liquor
industry. For the production of suitable enzymes the natural
changes which occur in the sprouting of seeds are used. The
employment of this natural chemical process is called malting,
and the product, malt.
Malt. Malt may be made from any cereal but is commonly
made from barley and unless otherwise specified, the term "malt"
is understood to refer to barley malt. The general preference
for barley is due to its high enzyme productivity, its ability to
retain its husk in threshing (husk subsequently serving as a filter-
ing material in the mash-tun) and the responsiveness of its endo-
sperm during growth to modifications and mellowing.
The following Figure 8 shows an enlarged cross-section of a
barley grain.
A grain of barley, or other cereal, consists essentially of two
parts, the main starchy portion, known as the endo-sperm and a
smaller part at one end of the corn known as the embryo. The
71
72 MALT
embryo is the rudimentary plant. From it rootlets eventually
develop which extract nourishment from the soil for the develop-
ment or growth of the plant. The rootlets do not appear in the
first stages and it is necessary for nature to provide some means
of feeding the embryonic plant. The nutrient media provided
by nature are principally starch, and smaller amounts of proteins
and other products. The nutrient materials are contained in the
endo-sperm and are insoluble and therefore non-diffusible through
the cellular structures to the germ where they are needed. Na-
ture has adjusted for this situation by providing that the plant
secretes certain substances, namely enzymes, very actively as soon
as germination commences. The enzyme, cytase, attacks the cellu-
lar wall structures and its action makes it possible for the enzyme,
diastase, to act upon the starch, changing it into a soluble form
and therefore rendering it diffusible, assimilable and available to
the germ as food. A portion of the insoluble proteins is also
acted upon and changed into soluble, diffusible and chemically
simpler substances, e.g., peptones, proteoses, and amino acids.
This change, commonly called proteolysis, is thought to be
brought about by other enzymes in the plant but little is definitely
known with respect to these agents, the action partly resembling
that of trypsin and partly that of pepsin or peptase. The actual
mechanism by means of which cytase enables the other enzymes
to reach the starch and proteins is also not definitely known; i.e.,
it is not known whether the cytase dissolves the cellulose or
whether its action is merely a softening one whereby the cellulose
MALT
73
is rendered permeable. Figure 9 is a diagram of the various
changes which take place within the grain during the malting
operation.
j Cellulose I
(envelopes^
\
GRAIN AT COMMENCEMENT
OF MALTING
CJ
c
j^
S
f Cytase |
< attacking >
cellulose I
. Diastase
f acts on starch 1
I and renders it I
I soluble, diffusible
I and assimilable. J
I Other enzymes act on *"|
proteins rendering them
soluble, diffusible and I
changing them to f
chemically simpler
substances. J
\
/Soluble starch and soluble
] products of proteolysis
I diffusing through grain to
I nourish embryo-
EMBRYO
GROWING
c
2
o
c
!c
|
6
Embryo's growth arrested
by heat from kiln
MALT
FIG. 9.
This is the process on which the maltster relies, but his en-
deavor is to keep the consumption of starch as low as possible
and hence when the action has proceeded to a point where he
judges the starch rendered soluble and the enzymes developed to
74 MALT
the most useful point the process is arrested and the plant killed by
drying the germinating grain in the malt kiln. This calls for
considerable judgment and experience on the part of the maltster,
but, in a general way, the end point may be said to have been
reached when the plumule has grown almost to the length of the
grain or corn. At this stage the starch should be in the proper
degree of conversion into sugar and the enzymes developed to
such a point as to be able to act upon and saccharify not only
the starch of the malt but also the starch of the unmalted cereal
with which it is often mixed in the mash tun. Since the yield
of alcohol is dependent upon the yield of starch converted to
sugar it is important to develop a malt of maximum diastatic
properties. It is also economical because it eliminates the neces-
sity of converting all of the cereal to malt.
Generally speaking, American malts have high diastatic
(starch-converting) power and are mixed with other cereals in
proportions ranging from 10 to 15 per cent of the whole for the
production of lower grade whiskies and from 20 to 50 per cent
for the higher grades. The United States Dispensatory requires
that malt shall be capable of converting not less than five times its
weight of starch into sugars. Distillers' malt, however, is usually
capable of accomplishing the conversion of nearly fifteen times its
weight.
Malt is used, either alone or in combination with unmalted
cereals, as a raw material in the manufacture of whiskey, gin,
vodka and kornbranntwein. It is also used as a raw material in
the manufacture of beer. It is, therefore, one of the most im-
portant products used by the liquor industry.
The finished product may be light yellow, yellowish-brown or
blackish-brown in color depending upon the intensity of the heat
treatment received in processing. Caramel malts are yellowish-
brown and are so called because they have been made from ordi-
nary malt submitted to a secondary process consisting of steeping,
drying and progressive heating until the sugar formed at the
lower temperatures is finally caramelized. Black malts are those
of the darkest color and are the product of comparatively high
temperature drying.
STEEPING 75
The malting operation offers several distinct advantages. It
assists in the development of the enzymes diastase, cytase and
peptase which are of great importance. It influences the solubility
of the albumen, starch and phosphates in the grains and affects
the condition of the starch for subsequent conversion in the mash-
ing operation.
Practical Malting. The malting operation consists in: i.
cleaning the grain, 2. adding water and steeping, 3. germinating,
Barley
Cleaning
Offal to
cattle feed-
dealers
- Water
Steeping
Skimmings dried and
sold to cattle feed
dealers
Germinating
Drying
Malt
Cleaning
Crushing
Finished Malt
FIG. 10.
4. drying, 5. cleaning and crushing. The sequence of these steps
is shown in the flow sheet, Figure 10.
Equipment and processes for cleaning, steeping and drying
are more or less standardized but various methods are available
for carrying out the germinating operation.
Steeping. This consists of soaking the cereal in water for
approximately 48 hours. Allowance must be made for variables
such as kind and condition of barley, water temperature, hard-
ness of water, humidity of air, etc. Float or ladle off skimmings.
Change the water every 12 hours the first day and every 24 hours
thereafter. When loading have tank half full of water and then
76 MALT
add barley, allowing water to stand i to 2 feet above the barley
when full. When cereal is properly steeped drain off water.
Germination. There are three methods available for carry-
ing out the germinating operation on a large scale. These are
respectively known as the floor, compartment, and drum systems.
The floor method was the first used, the other two representing
the contributions of modern chemical engineering. They are com-
monly referred to as pneumatic malting and are based on mechan-
ical as compared to hand turning over the grain and on subjecting
it to a flow of conditioned air either intermittently or continuously
during the raking or tumbling. Pneumatic malting is of great
assistance to the patent still distilleries; it permits all-year-round
malting.
Floor system. In this method the damp cereal is spread upon
the floor and is periodically shovelled over to aerate the germinat-
ing mass and keep its temperature below the scorching or burning
point. The right air temperature is about 60 F. and the grain
temperature should be about 75 F.
This part of the process must be watched closely and its suc-
cess depends on the judgment and experience of the maltster who
varies the depth of the grain at each working over. He will
usually start with a depth of about 8 to 10 inches and then alter-
nately and gradually increase and reduce it from a maximum of
14 inches to a minimum of about 5 inches.
Germination proceeds and in a few days reaches a point where
further growth must be arrested. This is usually when the leaf
or acrospire has grown to the length of the kernel. The ger-
mination is stopped by drying the green malt in the kiln. Man-
churian barley reaches this point in about five days while the
two-rowed and Bay Brewing types take about eight days.
Drum system. These are large drums of the rotating, tum-
bling type found in many chemical and other industrial plants.
They are arranged for continuous admission of conditioned air
and their speed can be varied to suit operating requirements.
It is customary to revolve the drums very slowly at first but,
as germination proceeds, the speed of rotation is gradually stepped
up. No definite operating rules can be set up since germinating
GERMINATION 77
conditions are never absolutely standard, but the following pro-
cedure may be used as a guide : twelve complete revolutions every
twenty-four hours for the first three days, then change to a full
revolution every hour and a half for the next thirty-six hours
and thereafter speed up to one revolution every forty minutes
until germination reaches the arrestation point in about twelve
hours more.
Compartment system. This consists of an oblong tank with
perforated bottom, usually of galvanized steel. The conditioned
air can be either top or bottom delivered. A carriage fitted with
revolving helices for stirring the grain travels across the top of
the tank and a sprinkling device is usually provided for moistening
the grain as it is turned over. Unloading is accomplished by
means of a scraper which draws the grain to one end of the tank
where an automatic device is located for feeding the germinating
mass to a conveyor.
Kiln drying. This is carried out in a three-storied building
fitted with a suction fan on the top floor and a furnace on the
ground floor. The furnace is fed with smokeless coal and air
and the hot gases are sucked up through the floors and exhausted
from the top of the building by the fan. The grain is spread
on the top floor and given a preliminary drying. It is then
dropped to the second floor where it is gradually subjected to
higher temperatures. This is an operation of some delicacy, and
considerable care and experience are required in order that the
malt may be dried gradually and not spoiled by scorching. Ex-
posing the green malt to too high temperatures at the beginning
of the drying operation will reduce its diastatic strength. For the
first 24 hours 90 F. is about right and it should then be dry to
the touch; thereafter the heat is gradually increased until a tem-
perature of 120 to 130 F. is reached in the 4Oth to 48th hours.
The maximum diastatic properties of the malt are obtained
when the drying is stopped at about 123 F. and this is an im-
portant point for the distiller of mixed mashes. Malts dried at
temperatures no higher than this point are usually referred to as
green malts.
On the other hand, where high diastatic power is not so
78 MALT
essential, as at all-malt distilleries, it is better to continue drying
to a higher temperature. This gives the following advantages:
( i ) a more friable product, easier to grind, (2) more suitable for
storage and (3) better fermentations and superior flavoring
properties. Offsetting these favorable characteristics is the fact
that green malts are more nourishing to yeasts and have about
ten times more diastatic power. Barley gives a malt of the high-
est diastatic power with rye, wheat, oats and corn following in
the order named.
Yield. After the malting and kilning operations the acreened
malt produced will weigh approximately 20 per cent less than the
green grain, but, taken by measure, the malt will exceed the origi-
nal grain by 6 or 7 per cent This is to say, the malt produced
is bulkier but less dense than the original green grain.
Acid Conversion. The theory of the acid conversion of
starch into sugars was discussed in Chapter I. Practically, this
method finds some use in the preparation of cereal raw materials
prior to fermentation although probably less in this country than
abroad. In the United States the hydrolysis of starch for fer-
mentation is almost invariably accomplished by the diastatic action
of malts. These malts are mixed with unmalted grain (the starch
of which has been pastified by prior cooking) and the conversion
to fermentable sugar carried to completion by a subsequent
operation called "mashing."
In Great Britain there is more variation in the means em-
ployed to secure a completely fermentable mash. There is first
of all the common process in which all of the diastatic action
comes from malt. Then there are two processes for making
mixed mashes. In the first of these, mixtures are made of malt
and unmalted grain, the starch of the latter having been com-
pletely converted by the acid process. In the second process the
action of the acid on the unmalted grain is halted before com-
pletion and a small proportion of malt added to finish the task
of hydrolysis. The preparation of these mashes will be discussed
again under the general subject of the whiskies prepared from
them.
CHAPTER VIII
DISTILLATION
Definitions. Distillation is defined as the separation of the
constituents of a liquid mixture by partial vaporization of the
mixture and separate recovery of the vapor and the residue. The
more volatile constituents of the original mixture are obtained in
increased concentration in the vapor; the less volatile remaining in
greater concentration in the residue. The apparatus in which this
process is carried on is called a still. Generally speaking, the
essential parts of a still are: i. The kettle in which vaporization
is effected, 2. the connecting tube which conveys the vapors to
3. the condenser in which the vapors are reliquefied. Modifica-
tions involving the addition of other parts to the still are intro-
duced for various purposes such as the conservation of heat and
to effect rectification. Rectification is a distillation carried out in
such a way that the vapor rising from a still comes into contact
with a condensed portion of the vapor previously evolved from
the same still. A transfer of material and an interchange of heat
result from this contact, thereby securing a greater enrichment of
the vapor in the more volatile components than could be secured
with a single distillation operation using the same amount of
heat. The condensed vapors, returning to accomplish this object,
are called "reflux" (The above definitions are substantially
based on "The Chemical Engineers 1 Handbook" by Perry,
p. 1 107-8.)
In less precise language, a simple distillation is a means of
separating a volatile liquid from a non-volatile residue. A frac-
tional distillation is a means of separating liquids of different
volatility. This latter process rests on the fact that no two liquids
of different chemical composition have the same vapor pressure
at all temperatures, nor very often the same boiling point.
79
8o
DISTILLATION
On the other hand, while its actual amount may be almost
vanishingly small, every liquid or even solid substance has a defi-
nite vapor pressure at any given temperature. Furthermore, that
vapor pressure is unchangeable at a fixed temperature by any
external means, but only by a change in the composition of the
liquid. From this it seems probable that the vapor pressure de-
pends partly on the nature of the liquid molecules and partly on
their mutual attraction. We have neither need nor space here
to develop the proof of this theory. Its application is as follows:
The molecules of water (B. P. 100 C.) and of alcohol
(B. P. 78.3 C.) do possess a strong attraction for each other
as shown by the contraction which is readily observed when the
BOILING POINTS OF ALCOHOL WATER MIXTURES
100 C C
78.30
78.17
Alcohol 100%
Water
_ i 50_
Alcohol 0%
Water 100%
FIG. ioa.
two liquids are mixed. The effect of this on the vapor pressure
and hence on the boiling point is shown in Figure ioa. From this
diagram, the proportions of which are exaggerated, it will be
noted that a mixture containing approximately 95% of alcohol
to 5% of water by volume has a lower boiling point (i.e., higher
vapor pressure) than either pure compound. From this it fol-
lows that alcohol higher than 95.57% cannot be produced by
distillation and also that in a simple still, starting with a mix-
ture of alcohol and water of relatively low alcoholic strength,
the first distillate will be higher in alcohol content and as the dis-
tillation continues the alcohol content of each succeeding portion
of distillate will be lower until finally pure water comes over.
The relation between the alcohol content of the first vapors and
distillate and that of the original boiling liquid as determined by
DEFINITIONS
81
Sorel (Distillation et rectification industrially 1899) is shown in
Figure lob.
If the first portion of distillate were condensed and redis-
tilled, the new distillate would be still richer in alcohol. For
instance, if the liquid being distilled contained 10% of alcohol,
the first distillate would contain 48.6% and this if condensed and
redistilled would contain 69-70% alcohol. Obviously, a practical
operation cannot be conducted in this manner. What is done,
therefore, is to introduce into the head of the still a number of
plates in each of which a portion of the vapor is condensed, yield-
ing a liquid somewhat richer in alcohol than the original liquid,
and this is again partly evaporated so that as we ascend the
O iuu
on
1
I
x
90
u>
| 80
= 70
_
^-
^
^
.-^
^
bU
>50
l_
-^
___
^^
.___
40
/
._
c
f
*30
/
-
o o n
/
j= -i n
o
< n
10 20 30 40 50 60 70 80 90 100
Alcohol Content of Liquid in Weight %
FIG. iob.
column each plate is progressively of higher alcoholic strength.
It is possible by the application of experimental results such as
Sorel's (loc. cit.) to these considerations to calculate the number
of plates required, and the proportion of condensate return re-
quired, to produce alcohol of any desired strength from a given
dilute supply. In general it can be seen that there is an inverse
ratio between the number of plates and the amount of reflux so
that as a practical matter it is advisable to increase the number
of plates as far as economically feasible in order to economize
fuel.
The fact that it is difficult to secure alcohol concentrations in
excess of 12-14% by fermentation alone, requires that for the
82 DISTILLATION
production of stronger liquors the process of distillation be ap-
plied. The increase in alcohol concentration which can be
achieved thereby depends on the effectiveness of the rectification
and the completeness with which it is desired to recover all the
alcohol. It can range up to a recovery in excess of 99% an d
alcohol of 95% strength by volume. The type and size of still
FIG. ii. Simple pot still used in liqueur manufacture.
actually employed in the distilled liquor industry depends on the
industrial development of the country in which the process is
being applied, upon the beverage being made, the raw materials
used, and the amount of material being processed at one time.
The various types may be classified as pot stills, Coffey or patent
stills, vat stills and continuous stills.
POT STILLS 83
Pot Stills. The simplest form of pot still is used in the man-
ufacture of liqueurs both on account of the small lots which are
worked and the method of manufacture. Such a still is shown
in Figure 11. "A" is the kettle; "D" is the "swan's neck" for
conveying the vapors to "R" the condenser; and "S" is the worm.
The mode of operation of this apparatus is obvious from an
inspection of the figure.
FIG. 12. Pot still used in French brandy manufacture.
C is the chauffe-vin used for pre-heating the wine fed to the still.
R is the condenser.
Figures 12 and 13 illustrate the addition of another part to
the simple pot still as used in France for the production of brandy.
This is the device marked "C," called in French the "chauffe-
vin," from its function of pre-heating the wine which is fed to
the kettle "A." This pre-heating is a mode of conserving some
of the latent heat of the vapors by passing them through the feed
84 DISTILLATION
to the kettle before leading them to the condenser. The types
of still illustrated are specially designed for brandy manufacture
and their peculiar adaptation for this purpose will be found in the
chapter on Brandy.
Improved Pot Still. In Great Britain the chief distilled
liquor is whiskey. Some of this continues to be made in pot-stills
FIG. 13. French brandy still fitted with chauffe-vin.
A is the kettle.
C the chauffe-vin.
R the condenser.
of somewhat improved design and considerably larger size as
shown in Figure 14. The pot stills used for this purpose are
divided into two classes, wash stills and low-wines stills. The
mash in which fermentation is complete, now called "wash," is
distilled in the former. The distilled product, low wines, is ap-
proximately a third of the volume of the original wash and
IMPROVED POT STILL
FIG. 14.
FIG. 15.
86
DISTILLATION
somewhere in the neighborhood of 25% alcoholic concentration.
Since a large volume of wash must be handled to produce a much
smaller volume of whiskey, the wash stills are very large, ranging
FIG. 1 6.
from 7,000 to 12,000 gallons capacity. It is not safe practice,
however, to charge these stills beyond 50-75% of their capacity,
to avoid foaming and priming, that is, the carrying over of some
FIG. 17.
of the boiling wash into the condenser. A still of the size range
indicated may be expected to distill about 600 gallons of wash to
low wines per hour.
Figure 15 is an improved pot still, arranged for direct firing
and equipped with a rectifier in addition. The vapors pass from
the kettle into the rectifier, which is similar to an ordinary con-
COFFEY STILL 87
denser. The least volatile portions are condensed and returned
to the still. The more volatile portions of the vapor pass on to
the regular condenser.
A doubling of this arrangement is shown in Figure 16. This
kind of equipment is used in the British West Indies for the
production of rum. Either Figure 15 or 1 6 may also be arranged
for heating by steam instead of direct firing.
Another type of rectifying arrangement called a "Corty's
head" is shown in Figure 17. Four traps are fitted into the neck
of the still. Each trap contains a diaphragm by means of which
the direction of the rising vapors is changed, forcing them to
circulate around the trap. Cooling water enters the system by
means of the pipe (9) and flows downwards through pipes (10)
from trap to trap. A fractional condensation occurs in each trap
causing progressive rectification of the ascending vapors in an
effective manner and resulting in the vapors passing to the total
condenser being much richer in alcohol than those evolving from
the boiling liquid in the kettle.
Coff ey Still. The Blair, Campbell and McLean form of the
"Coffey" or patent still, shown in Figure 18 in plan, and
diagrammatically in Figure 19, is a much more effective rectify-
ing and distilling equipment. Instead of applying direct heat
to a large volume of wash in a kettle, the wash is spread
in thin layers over a large surface and heat supplied by
the introduction of steam from an external boiler. The wash
enters the still at the top and trickles down over a series of per-
forated copper plates. Steam enters the still at the bottom and
bubbles upward through the perforations, each of which is in
effect a trap. By this means the wash is heated and the alcohol
vaporized so that by the time the wash has reached the lowest
plate it has lost all of its alcohol and can be discharged from the
still with its dissolved and suspended solids. As the mixture of
alcohol vapor, volatile impurities, and steam rises toward the top
of the apparatus, the lower becomes its boiling point, more steam
is condensed from it, and the richer it becomes in alcohol. The
part of the still in which this operation takes place is called the
"analyzer."
88
DISTILLATION
FIG. 1 8. (From Martin Industrial and Manufacturing Chemistry-Organic, Crosby,
Lockwood and Son, London.)
COFFEY STILL
89
90 DISTILLATION
The vapors from the top of the "analyzer" are led into the
bottom of a second column of perforated plates which is called
the "rectifier." There is a zig-zag tube full of cooling liquid
extending the full length of this column to serve as a condenser.
Usually cold wash on the way to the analyzer is employed as
cooling liquor, while it is thereby preheated, thus effecting econ-
omy of heat. The alcoholic vapors on their upward passage
through the plates are fractionally condensed in each cooling
chamber and lose their water until finally they are condensed on
an unperf orated sheet at the top of the column (the "spirit
plate") as very strong alcohol, and are removed. It is stated
that from 94-96% spirit can be continuously obtained from this
type of still, whereas a simple still at best and even by repeated
distillations will only yield a small quantity of strong alcohol not
over 90-92% by volume from each operation.
A mixture of weak, impure alcohol and "fusel oil" ("hot
feints") collects in the bottom of the "rectifier." This is re-
turned to the "analyzer" to recover the alcohol. Towards the
end of the distillation of a batch, however, instead of completing
the purification of all the alcohol, it is found more economical to
raise the temperature of the apparatus and distill off the whole
residue of impure spirit. This is condensed and collected as
"feints" in a separate receiver. Here the fusel oil which has
accumulated throughout the process separates, to a large extent,
from the weak spirit and is skimmed off. The remaining
"feints" are redistilled with the wash of a succeeding operation
to recover their ethyl alcohol.
In the United States alcohol is distilled and rectified from its
wash by means of continuous stills. In smaller establishments all
non-volatile materials and a substantial portion of the water are
removed in a so-called "beer still," Figure 20. On account of the
partial rectification in the preheater the distillate from a 6%
beer will frequently run as high as 40 to 60 per cent alcohol.
The crude alcohol is neutralized with some suitable alkali such
as soda ash, and then purified and concentrated in an intermit-
tent still, Figure 21. Assuming that the feed runs as high as
60 per cent alcohol, the feed is diluted so as to reduce the con-
COFFEY STILL 91
centration to 50 per cent and the distillate will run as high as 95
per cent alcohol but is collected in a number of portions of which
70 to 75 per cent can be used as spirits. The neutralization of
the distillate from the beer still must be very carefully done,
because if the solution is boiled when alkaline, the nitrogenous
Steam =W= xnz
FIG. 20. Beer Still. (Redrawn from Robinson's Fractional Distillation. Courtesy
McGraw-Hill Book Co., Inc.)
bodies set free amines whose disagreeable odor is difficult to
remove in the finished alcohol, and which also form blue com-
pounds with copper which discolor the alcohol. Another draw-
back is that they tend to combine with the aldehydes, forming
resins which may gum up the column, or impart a yellow color
to the alcohol withdrawn from the column. On the other hand,
92 DISTILLATION
if the solution is acid, esters will form, and any undecomposed
ammonium acetate will react with strong alcohol forming ethyl
acetate and setting free ammonia. (See Robinson, u The Ele-
ments of Fractional Distillation.")
The operation of the beer still shown in Figure 20 is per-
formed as follows : The alcoholic feed is supplied by a constant
level feed tank "A" containing a ball float which controls a steam
Dephlegmator Condenser
Column
Kettle
rr - -
u
-U
Steam I
T
FIG. 21. Intermittent Still (modern). (Redrawn from Robinson's Fractional Distil-
lation. Courtesy McGraw-Hill Book Co., Inc.)
pump to pump the feed from the storage tank to A as rapidly
as it is used. The feed then flows by gravity through the feed
heater "B" where it is raised nearly to its boiling point. Con-
tinuous stills are often fitted with recuperators in which the in-
coming feed is heated by the outgoing hot waste from the bottom
of the exhausting column. If the liquor contains solid materials
that are likely to form deposits on the heating surfaces, recupera-
tors are dispensed with, on account of the difficulty of cleaning
the outside of the tubes. The vapor heater shown at "B M has
COFFEY STILL 93
the liquor only inside of the tubes, and the fouled surfaces can
very easily be cleaned by removing the top and bottom heads of
the heater, and passing a cleaning device through the tubes.
The hot feed is introduced into the top section of the exhaust-
ing column "C" where it flows downward from plate to plate;
the volatile portions are gradually removed as the liquor comes
into contact with the steam blown in at the bottom through the
perforated sparger pipe "L." The exhausting column has usu-
ally from 12 to 15 plates, each plate being large and deep to
give a long time of contact of the feed in the column in order to
insure complete removal of the volatile substances. The com-
plete removal of these substances is readily tested by what is
known as the slop tester. Vapor is withdrawn from a plate near
the bottom at "H," any entrained liquid removed by the separat-
ing bottle, and the vapor condensed in a suitable condenser "I,"
from which it flows to a tester "J" where it can be tested, or its
specific gravity measured by means of a hydrometer. The
exhausted liquor is then discharged from the bottom of the still
through a suitable seal pipe "M. n The rate of introduction of
steam into the column is governed by means of a suitable pressure
regulator.
The vapor leaving the exhausting column to pass to the heater
is substantially in equilibrium with the liquid on the top plate of
the column. It is partially condensed in the heater, enriched in
its alcohol content, and then passes to the condenser where it is
completely condensed. The portion of the vapor condensed in
the heater is returned to the top plate of the column together
with a controlled portion of the vapor condensed in the con-
denser, from the regulating bottle "E." The distillate flows,
through the tester "F" where its quantity and specific gravity
may be measured, to the storage tank "G." The water supply
for the condenser is obtained from the constant level feed
tank "N."
In larger establishments a continuous rectifying still is used in
place of the intermittent still for the second operation. Figure 22
is a diagram of such a continuous rectifying still. The still con-
sists essentially of a purifying column "C" and a concentrating
94
DISTILLATION
and exhausting column "D." The function of the purifying
column is to remove the volatile head products, which are sep-
arated from the alcohol by fractionation. The function of the
concentrating column is to separate the alcohol from water, as
well as from the less volatile impurities which are not removed
in the heads. This rectifying unit will produce an alcohol of
higher grade than the best produced by the intermittent still with
FIG. 22. Ethyl Alcohol Still (continuous). (Redrawn from Robinson's Fractional
Distillation. Courtesy McGraw-Hill Book Co., Inc.)
a recovery of perhaps 75 to 85 per cent. It will avoid the neces-
sity of subsequent purifying treatments with charcoal, etc., and
rehandling of intermediate fractions at a considerable saving in
time, labor, and expense. The purifying column is fitted with a
partial reflux condenser "G" and a total condenser "H" and is
independent of the rest of the apparatus except that it receives
the hot feed continuously from the recuperator "B" and the
feed supply tank "A" and delivers the purified dilute alcohol con-
tinuously from its base to the other column "D." It has its own
COFFEY STILL 95
steam regulator "O" and cooling water supply and its rate of
operation can be controlled according to the amount of the im-
purities to be removed.
A further improvement of this system of alcohol production
is shown in the plan in Chapter IX on Whiskey. Here the beer
still is connected directly to the rectifying unit so that the feed
to the rectifier is in the form of a vapor instead of a liquid. This
effects considerable saving of steam for heating purposes and the
final product contains not less than 98 per cent of all the alcohol
present in 'the beer and produces 90 per cent of this alcohol as
high grade, pure spirits, the remainder as heads, and a washed
fusel oil. Chemical analysis cannot determine whether the al-
cohol produced comes from molasses or grain. These units use
about 40 pounds of steam per gallon of alcohol produced. Fur-
ther improvements now pending will give an even higher yield.
The most modern American whiskey still consists of a column
and an extra head which contains two rectifying plates and one
washing plate. This still and its mode of operation are described
in Chapter IX on Whiskey.
CHAPTER IX
WHISKEY MANUFACTURE
Historical. Whiskey is essentially an English and American
beverage. It was first developed in the United Kingdom and
subsequently its manufacture was taken up in this country.
When whiskey was first made is not definitely known. But
Usquebagh (from which the word "whiskey" derives) is said to
have been made in Ireland in the twelfth century and it is re-
ported that its manufacture there had assumed sizable propor-
tions even before Queen Elizabeth's time. It is also said that
distilled spirits were made by the monks prior to the fifteenth
century and that they jealously guarded the secrets of their form-
ulae and methods of manufacture. However, commencing with
the fifteenth century the process became more widely known.
There is a treatise on distillation which is one of the very first
of printed books. At first the manufacture was carried on in
a small way in the household, but a young whiskey distilling in-
dustry was gradually established. At that time spirits were made
from malt in Scotland and from wort and sour beer in England.
The industry was operated under government supervision in all
three countries and its products were taxed. As a result, the
history of spirit distilling can be followed fairly accurately by a
study of the taxation legislation.
The industry has had a very stormy career and it is interest-
ing to note that in the sixteenth, seventeenth and eighteenth cen-
turies many of its troubled periods and their subsequent develop-
ments paralleled conditions under the prohibition era in the
United States in the last thirteen or fourteen years. For example,
restrictive legislation, high taxation, manufacture under strict
government supervision and last, but not least, the bootlegger, or
96
HISTORICAL 97
as he was then called, the illicit distiller, all existed long before
our times. Smuggling was often rife, and England had its rum
row two or three hundred years before America. In 1556 there
was a death penalty in Ireland for illicit distillation.
In the reign of Charles I there was formed the Distillers*
Company of London, which received a charter of incorporation
and was empowered to regulate the manufacture of whiskey from
the point of the quality of materials to be used. A little later,
in the reign of Charles II, distilling materials included such
varied substances as sugar, molasses, sour wines, sour ales, cider,
and wort from grain and malt; and the products included whiskey,
brandy, gin, and rum (although much of this was made in
Jamaica). By 1694 annual production in England had risen to
900,000 gallons.
The seventeenth, eighteenth and nineteenth centuries were
periods of experimental taxation and other governmental regula-
tion in Scotland, England, and Ireland, and the industry may be
said to have grown in spite of, rather than because of, these
regulations. Prior to 1860 the taxation and regulations were
different in all three countries; and in Scotland, during one period,
there was even a wide difference in regulations for Lowland and
Highland distilleries. At one time taxes were either collected by
local authorities or were farmed out to private persons or busi-
ness houses, who received a percentage of their collections for
their services. It was quite common for such tax collecting con-
tracts to be let and sub-let. Later, a fixed minimum of receipts
was stipulated for each distilling region. Following this another
form of taxation was tried, based on the capacity of the still and
its rate of operation, but the legitimate distillers displayed con-
siderable ingenuity in beating the law, often by faster distilla-
tion. Morewood (Inventions, etc., in Intoxicating Liquors,
1824) describes a still for this purpose which was built with
the unique proportions of 48 inches in diameter and only three or
four inches deep!
Thus, three centuries have passed and a satisfactory solution
of the problem is still sought. When taxation was high and
regulations very restrictive, legitimate production waned and il-
98 WHISKEY MANUFACTURE
licit distillation and smuggling increased. When taxation was
lowered and regulations made less restrictive, legitimate manu-
facture would prosper and smuggling and illicit manufacture
diminish.
In 1730 the laws almost killed the industry, but illicit distilling
became so profitable that the government was forced to revise
the regulations in 1743. Legitimate production then jumped to
5,000,000 gallons of proof spirit In 1751, and again in 1756,
taxation was increased and legitimate production gradually
dropped till it amounted only to 3,000,000 gallons in 1820. In
1760, 500,000 gallons of spirit were smuggled into England
from Scotland. About the year 1800, 6,000 illicit stills were
seized in Ireland in one year and illicit production exceeded legiti-
mate production three or four times. Taxation was revised in
Scotland in 1817, and in England in 1823, and finally in 1860 all
legislation was consolidated and restrictions were somewhat re-
laxed. Since then further concessions have been made from time
to time, the greatest being those since the war. At present the
tax is about $2.00 per bottle.
The history of whiskey manufacture in the United States is
not so easily traced. The date of the building of the first distil-
lery is uncertain, as is the progress of the industry in the eight-
eenth and nineteenth centuries. However, no book on this sub-
ject can omit a reference to the "Whiskey Insurrection 77 which
occured in Western Pennsylvania in 1792 to 1794, when Presi-
dent Washington was compelled to call out the militia to quell
the insurrectionists, so strong was the reaction against the excise
regulations put into force about that time.
The prohibition question, especially its legislation and devel-
opments in the past two decades in the United States are too well
known to warrant reviewing. According to D. S. Bliss, U. S.
Commissioner of Industrial Alcohol, only seven distilleries were
legally operated during this period for the purpose of manufac-
turing whiskey for medicinal purposes. They were allowed to
manufacture only limited quantities and they started operation
during the fall of 1929. On the manufacture of whiskey during
the last three decades see also Chapter XV on Statistics.
DEFINITION AND TYPES 99
Definition and Types. Whiskey may be defined as an alco-
holic beverage produced from cereal grains by the following gen-
eral series of operations:
1. Transformation of the starch of the grains, either malted, unmalted,
or mixed, into fermentable sugar.
2. Fermentation of the sugar to produce alcohol.
3. Distillation to concentrate the alcohol.
4. Ripening by aging in oak barrels.
There are available on the market a number of types of
whiskey, which as the result of variations in the details of proc-
essing or in the raw materials used, possess different flavors and
other characteristics of importance to the consumer. In general
these may be classified as :
American
Rye:
Made from a mash composed of unmalted rye and either rye
or barley malt.
Bourbon :
Made from a mash composed of maize and either wheat or
barley malt.
Low grade American whiskeys are made from mashes con-
taining from i o to 15 per cent malt.
High grade American whiskeys are made from mashes con-
taining from 20 to 50 per cent malt.
Most American whiskeys are made in patent stills.
Scotch
Pot still:
Made from barley malt and having a smoky taste, obtained by
using peat instead of coal as fuel in the kiln drying of the malt.
Changes in the variety of peat used materially affect the flavor.
This includes scotch whiskeys commonly classified in the British
Isles as follows: (i) Highland malts, (2) Lowland malts,
(3) Campbelltowns, (4) Islays.
Patent still :
Made from a mash composed of unmalted cereals and barley
malt. The former may be either rye or oats but commonly is
American maize (corn). These whiskeys do not have the
smoky taste and are more American in character.
ioo WHISKEY MANUFACTURE
Irish
Pot still :
Made from an all-malt mash or from a mixed mash composed
of barley malt and unmalted cereals. The latter may be barley,
oats, wheat, rye or variously proportioned mixtures. Malt runs
high, from 30 to 50 per cent of the whole.
Patent still :
Made from a mash composed of unmalted cereals and barley
malt.
On a different basis all mixed mash whiskies may be classi-
fied as either:
Sour or sweet mash
Sour mash:
A whiskey made by cooking the ground, unmalted cereal with
spent liquor of a previous mash which has been dealcoholized by
distillation.
Sweet mash :
A whiskey made by cooking the ground unmalted cereal in the
ordinary way with water.
Blends. In addition to the straight whiskeys described above,
both in this country and abroad various blends have come into
public favor. Especially in Great Britain blending has become
a very large trade as it is stated that the public taste demands a
whiskey of less prominent but more uniform characteristics than
formerly. To gratify this desire blends are made, in the United
States presumably of straight whiskeys; but in Great Britain
either by the mixture of various pot still whiskies of varying age,
etc., with the possible addition of silent spirits from patent stills.
In the latter case cheapness is often the purpose of the blend,
but it is also stated that it unites the several whiskies in the mix-
ture more completely and enables the blender to produce a whis-
key of more uniform character. Blends, even when made from
aged spirits of various kinds, are frequently stored in bond for
considerable time. The addition of patent still spirits, even those
containing very small amounts of secondary products, is viewed
as dilution rather than as adulteration. Methods of blending are
discussed under that heading later in this chapter.
MASHING 101
MANUFACTURE OF WHISKEY
General Outline. The manufacture of whiskey is essentially
a chemical process based on changes in the composition of ma-
terials brought about by temperature alterations and the effect of
the activity of ferments and other reagents. Very little depends
on mechanical manipulation and there is a lack of spectacular
features.
Successful operation depends on a complete understanding of
the changes taking place in the composition of the materials and
on accurate temperature control. Technical knowledge, experi-
ence and judgment are required to select and control conditions
and materials so that a high yield of uniform product is obtained.
It has Seen the object of the preceding chapters to explain
the theoretical bases on which the process of whiskey making
rests. In the present chapter the sequence of the operations and
some of the manners of control are discussed. In actual fact,
it is very easy to make a sort of crude whiskey by simple perform-
ance in regular order of the first three or four basic operations
listed in this chapter in the section on definitions and types. The
commercial production of whiskey in quantities is very largely a
magnification in scale of these operations with the introduction of
refinements and modifications designed to facilitate the opera-
tion, secure a more uniform product, and obtain a maximum
yield. It is to be expected, therefore, that the historical steps in
the change from the simple u home still" of earliest times to the
largest scale continuous operation of American practice have
been preserved and can be seen in the manufacture of whiskey in
various establishments in different countries. This is the case
to such an extent that the common varieties of whiskey are each
identified with a different degree of evolution in the whiskey
making process. A number of distinct process sequences can be
formulated on this basis, of which the following are outstanding.
(See Table VIII).
Mashing. In all types of whiskey, the process, by which all
the starch of the grains used is brought into solution, is called
mashing. It involves both extraction and conversion of the starch
102 WHISKEY MANUFACTURE
TABLE VIII. TABULAR COMPARISON OF WHISKEY PROCESSES
Whiskey
type
Materials
Scotch or
Irish
All malt
Scotch or
Irish
Scotch or
Irish
American
small scale
American
large scale
Malt and
grain
Malt and
grain
Malt and
grain
Malt and
grain
Pre-m ashing
None
None
Partial acid
conversion
Cooking at
normal
pressure
High pressure
cooking of
grain
Filtration
of mash
Yes
Only wort is
fermented
Yes
Only wort is
fermented
Yes
Only wort is
fermented
No
Whole mash
is fermented
No
Whole mash
is fermented
Method of
distillation
Pot still
Pot still
Patent still
Patent still
Patent still
into sugars. The process is carried out in an apparatus called a
u mash tun" as illustrated in Figure 22a. The essential parts of
a mash tun are a vat equipped either with steam coils or means
FIG. 223. Mash tun and apparatus. (Redrawn from Rogers* Manual of Industrial
Chemistry, D. Van Nostrand Company, Inc.)
of heating by direct injection of steam, and an efficient agitator.
The latter must have both scraper and stirrer arms to ensure that
all the ground grain comes into contact with the water.
SCOTCH OR IRISH POT STILL WHISKEY 103
Water. The quality of water used in mashing is very im-
portant both on account of its influence on the quality of the
finished liquor and in its own right, since it is used by the distiller
in many times greater volume than any other of his materials.
As used in mashing it is possible for impurities in the water to
cause irreparable damage. It is also claimed that the water used
influences the flavor of the finished whiskey. There is even told a
tale of a Scotch distillery being built on the banks of a stream and
then abandoned and a new distillery built on another stream
twenty miles away because the water from the latter resulted in a
product of superior flavor. As the Italians say Se non e vero, e
ben trovato. Certainly it is known that Scotch and Irish distil-
lers emphasize greatly the purity of their water supply. They
select by preference, moss water, or some special location such
as Loch Katrine or the river Bush, whose name is part of the
trade name of "Old Bush Mills."
Lacking such ideal locations, an effective water purification
and softening plant may be necessary if the water supply is in
the least questionable. The magnitude of the problem is readily
seen from the fact that a pot still distillery, on a basis of 1,000
bushels of malt mashed weekly, will require about 240,000 gallons
of water, and a patent still distillery, producing 20,000 proof
gallons of alcohol per week, will use about 700,000 gallons of
water in its production.
Scotch or Irish Pot Still Whiskey. Preparation of Wort.
As can be seen from Table VIII (p. 102), the manufacture of
this type of whiskey involves the least introduction of modern
improved processes. The mashing procedure as shown diagram-
matically in Figure 23 consists of three extractions of the ground
grain, either all malted or a mixture of malted and unmalted, with
separate portions of liquor. Oat husks are added to assist in
the drainage or filtration of the wort and the third or final liquor
from one batch of grain is used as the first liquor on the succeed-
ing batch. The liquor is heated to the proper temperature, poured
over and mixed with the cereals in the mash tun, allowed to soak
for a suitable time and drained off. The first two liquors ob-
tained in this manner are cooled to the proper temperature for
IO4
WHISKEY MANUFACTURE
fermentation and run to the fermenting vats. The third liquor
or "weak wort" is returned for use on the next batch of malt.
Fermentation. This stage of the process of whiskey making
permits of only minor variations in methods of inoculation, time,
temperature control, etc. The general practice is the same both in
Oat husks to
facilitate
filtration
Ground Malt
Weak wort from
previous mash
I
Temperature
1 50-1 60 F
25-35 gal. per cwt.
of malt.
First Mashing
Initial temperature
135-145 F
Hot Water
Wort to coolers and
fermentation vat.
Second Mashing
*" 150-1 55 F
Hot Water
Wort to cooler and
fermentation vat.
Third Mashing
165-170F ,
Exhausted Mash to
waste or recovery
FIG. 23.
Weak wort to heater
and recirculation.
America and in the British Isles. The principles to be observed
have been outlined in Chapters III and VI.
The customary procedure is as follows : The wort coming
from the mash tuns, filtered abroad, unfiltered here, is cooled to
between 68 and 70 F. Yeast in a vigorous state of activity
is added and the fermentation proceeds. The temperature of
the fermenting liquor increases and must be carefully controlled
by passing cold water through coils in the fermentation vat. The
amount of temperature rise permitted has a direct effect on the
time of fermentation. In some distilleries the rise is kept small
SCOTCH OR IRISH POT STILL WHISKEY 105
and the fermentation slow. In most, however, the temperature
is allowed to advance about twenty degrees in the first twenty
hours. The temperature is never permitted, however, to exceed
90 F. Since the distillers' yeast is very active, a sweet rye fer-
mentation, for example, is usually complete in 72 hours.
It is observed that high and rapid fermentations on the one
hand are more likely to exhaust the sugar in the wort, but on the
other hand, it is claimed that they are responsible for the forma
tion of larger amounts of the congeneric substances including
esters, fusel oil and aldehydes.
deration. Some form of aeration is necessary both before
and during fermentation. It may vary from the simple raising
of buckets full of wort and pouring them back, to elaborate per-
forated pipe and air pump assemblies. The results of aeration
and the objects of the practice include: i. thorough stirring and
intermingling of wort and yeast, 2. maintenance of uniformity
of temperature throughout the vat, 3. expulsion of carbon diox-
ide from the wort, 4. stimulation of yeast in vigor and multiplica-
tion, 5. flocculation of suspended matter.
Distillation. On the conclusion of the fermentation, the
liquor, now called "wash," is ready for distillation. In Scotch
pot still practice two distillations are required for preparing whis-
key from the wash. The first takes place in the wash still. The
distillation is continued until all the alcohol has been driven off
from the wash and collected in one distillate. The liquor re-
maining in the still is termed "pot ale" or "burnt ale"; and is
either run to waste or dried for fertilizer. The distillate, which
is technically termed "low wines," contains all the alcohol and
secondary constituents from the wash, and considerable water.
The low wines are transferred to a second and smaller still and
arc redistilled. Three fractions are obtained from this distilla-
tion. The first is termed "foreshots," the second constitutes the
clean or finished whiskey, the third is called "feints." The fore-
shots and feints are collected together, while the residue in the
still, called "spent lees" is run to waste like the pot ale.
The judgment and experience of the distiller determine the
point at which the collection of foreshots is stopped, and that of
106 WHISKEY MANUFACTURE
whiskey commenced, and similarly that at which the latter is
stopped and the collection of feints begun.
The strength at which the whiskey fraction is run is of great
importance as regards the character of the spirit. In Scotland
this is generally from about n to 25 degrees over proof
(11-25 .p.)-
The foreshots and feints from one distillation are mixed and
added to the charge of low wines for the next distillation and so
throughout the distilling season. The feints collected from the
last distillation of the season are kept to be added to the low
wines from the first distillation of the succeeding season.
In some distilleries in Scotland the whiskey is produced in
three distillations. This practice is very general in the Low-
lands; the spirit being then run at 40 to 45 degrees over proof.
The volatile secondary constituents, which pass over with the
alcohol into the low wines receiver, on the distillation of the wash,
are thus incorporated as far as possible with the finished whiskey
finally produced. There can be no doubt, however, that a portion
escapes with the spent lees since it is known that partial decom-
position is undergone during the process of distillation, e.g., cer-
tain esters are easily decomposed when boiled with water under
such conditions as those which obtain during distillation in the
wash or low wines stills and the products of decomposition may
wholly or partially remain in the spent lees and may consequently
be absent from the whiskey.
Again, some of the constituents which boil at much higher
temperatures than water, may not wholly pass over with the
alcohol in the distillation of the low wines, but may remain in the
spent lees, and so also be lost to the finished whiskey.
The extent to which the loss of secondary constituents may
thus occur and affect the character of the whiskey depends largely
upon the variety of pot still employed, and the manner of its
operation; whether, for instance, the process of distillation be
carried on slowly or rapidly; and it also depends on the strength
at which the whiskey fraction is run.
In Irish pot still practice the stills employed differ somewhat
from those used in Scotland in that they are generally much
BRITISH PATENT STILL WHISKEY 107
larger, the wash still occasionally being of a capacity of 20,000
gallons. The head of the still is shorter and in the still used for
the distillation of low wines and feints the pipe connecting the
head of the still with the worm is of considerable length and
passes through a trough of water, the result being that a certain
amount of rectification of the spirit vapor is effected on its way
to the worm. This pipe is termed the "Lyne arm" and is con-
nected with the body of the still by what is known as a "return
pipe" through which is conveyed to the still for redistillation any
liquid which has condensed in the pipe.
Three distillations appear to be universally practiced in Ire-
land for obtaining pot still whiskey and the method of collecting
various fractions during a distillation is somewhat more compli-
cated than with the Scotch process. Strong low wines and weak
low wines, strong feints and weak feints, are collected and blended
in various orders, and the practices in this connection probably
differ in every Irish distillery. The whiskey fraction is usually
run at a higher strength than in the Scotch process, viz; from
25-50 per cent o.p.
The addition of charcoal and also of soap in distillation is
common both in Ireland and in Scotland, the soap being used to
prevent frothing in the wash still and the charcoal in the low wines
still to remove undesired constituents by absorption.
The differences between Scotch High and Lowland and Irish
practices in pot distillation are readily seen from the flow dia-
grams (Fig. 24).
British Patent Still Whiskey. General Statement. It is
claimed for patent still operation in preference to pot still opera-
tion that various economies are achieved as follows:
i . Economy of time :
a. Operation is continuous and rate of distillation is greater. There
is a continuous feed of wash and a continuous discharge of spent
wash, as compared with shut downs to charge and discharge in
pot still practice.
b. Rectification and distillation are carried out as part of the one
process, whereas in pot still practice rectification is only partially
achieved in one distillation, and two or even three distillations are
necessary for complete rectification.
io8
WHISKEY MANUFACTURE
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BRITISH PATENT STILL WHISKEY 109
c. Only one condensation of the distillates is necessary, with cooling
from a maximum temperature of 150 F. down to 60 or 70 F.,
as compared with pot still practice in which two or three con-
densations are necessary.
d. Operation can be carried on throughout the year.
2. Economy of operation:
a. Less cooling water required for condensing vapors to distillates.
b. Cold wash is used to condense vapors to distillate, and the latent
and sensible heats of the vapors and of the distillate serve to pre-
heat the wash and raise it almost to its boiling point. This
results in large fuel savings for primary heating.
3. Efficiency of operation:
a. Pure grain alcohol for use in the arts can be made as well as
alcohol for denaturing.
b. A highly rectified whiskey can be produced.
c. Distillate is 148 to 154% proof.
d. Strength of distillate can be practically constant despite wide
variations in strength of wash.
4. Miscellaneous:
a. A greater variety of materials can be used and from practically
all sources of supply so that advantage can be taken of temporary
low prices.
b. Yeast can be made as a by-product.
On the other hand, the elimination of secondary products con-
tained in the fermented wash is 95 per cent for the patent still
as compared to only 90 per cent for the pot still. Hence many
old time Irish and Scotch whiskey makers claim that it is the
presence of some of these secondary products in the distillate
which determines that their product is whiskey and not merely
"neutral spirit**; i.e., flavorless, pure grain alcohol.
The Scotch and Irish pot distillers claim that over a period
of many years they built up a world-wide reputation for a bever-
age called "whiskey" to obtain which it is necessary to distill a
wash, obtained from certain raw materials, in a pot still according
to certain methods developed by long years of practical research
and experimentation. They claim that no patent still spirit, how-
ever dosed with flavors, can duplicate the quality and flavor of
their product.
no WHISKEY MANUFACTURE
Preparation of Wort. In harmony with greater efficiency in
the distillation, patent still operators have introduced modifica-
tions in the method of saccharification of their cereal grains, usu-
ally by some application of the "acid-conversion" process. This
process has as its object partial conversion of the starch of the
grains into fermentable sugars by the use of acid rather than the
diastase of malt and depends on the latter only for the final com-
pletion of the conversion.
The general principles underlying this operation have been
discussed in Chapter I on Starch. In practice small amounts of
either sulphuric or hydrochloric (muriatic) acid are added to the
mixture of ground grain and water, heat is applied until the
action has proceeded to a sufficient extent and then the acid is
neutralized. The procedure consists in mixing in a tun about
36 gallons of water per cwt. of ground cereal or grist. About
1-1.5 pounds of 60 B. sulphuric acid (oil of vitriol) suitably
diluted (by pouring the acid into the water never the reverse) is
added for each cwt. of grist. Agitation is applied, and steam
injected so that the temperature rises gradually. Care must be
taken that the heating is neither too high nor too prolonged.
When the starch has been gelatinized and the whole converted to
a thin liquid the action is stopped by neutralizing the acid. Ordi-
narily milk of lime (a suspension of slaked lime in water) is used
to accomplish most of the neutralization and the rest effected to a
very faint acid reaction by the gradual addition of powdered
chalk. At the optimum condition of acidity cold water is added
to cool the batch to about 145 F.
The batch is then discharged into the mash tun in which
some malt at a temperature of I25-I3O F. has been previously
prepared. The temperature of the whole mash after mixing
should be about 138 F.
There are various modifications of this acid conversion proc-
ess in which small amounts of malt are added at different stages
to supplement the action of the acid. Three such variations are
shown diagrammatically in Figure 25.
It will be noted from Figure 25 that the first modification
represents the acid conversion process exactly as described prc-
BRITISH PATENT STILL WHISKEY
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s
ii2 WHISKEY MANUFACTURE
viously. In the second modification a small portion of malt is
added immediately to the ground cereal which is steeped in tepid
water. Heat by steam injection is carefully applied so that the
rate of temperature rise is very closely i F. per minute. The
acid is only added when the batch has heated up to i65-i7o F.
and the cooking is then continued as previously. In the third
modification it is customary to use more water (50 gal. per cwt.)
and less acid ( l / 2 Ib. per cwt.). The cooking follows the usual
procedure except that a small portion of malt is added to the acid
mash as a final step before it is poured into the main malt mash.
In each case three extractions on a sort of counter-current system
are used as in the all malt process.
Fermentation. While equipment in a patent still distillery
may be both larger and more elaborate, the process of fermenta-
tion is practically identical with that described under pot still
whiskey (p. 104).
Distillation. The operation of a patent still in the British
Isles is in all respects as described in Chapter VIII and on page
126 of this Chapter under American Practice. The wash or
beer is fed continuously from a storage tank or well through a
heater, in which it absorbs heat from the ascending spirit vapors,
into a distilling column consisting of perforated plates. Steam is
fed at the bottom of the still causing evaporation of alcohol from
the wash. By regulation of:
1. Rate of beer inflow
2. Point of beer entry
3. Steam input
4. Amount of condensed vapor returned to column (reflux)
5. Point of reflux entry
a dynamic equilibrium is established within the still. That is, the
temperature and concentration of liquid at each point of the still
remain constant even though there is continuous counter-current
flow of liquid and vapor past the plates. Hence, it becomes pos-
sible to discharge from the still bottom a spent slop containing
less than i per cent of its original alcohol and to recover over
90 per cent of the alcohol as whiskey of 50-75 per cent o.p. and
BRITISH PATENT STILL WHISKEY 113
of almost any desired content of the "congeneric substances" on
which the flavor and odor depend.
Operation and Yield. Nettleton ("The Manufacture of
Whiskey and Plain Spirit" Aberdeen, 1913) cites records of
various distilling operations at pot and patent still distilleries
from which the following have been abstracted for comparison :
LOWLAND POT STILL DISTILLERY ALL MALT
Equipment :
2 wash stills, each 6,200 gallons capacity
2 low wines stills, each 3,800 gallons capacity
Batch:
2,600 bushels of malt 835 cwt. malt
Wash:
54,100 gallons
4 consecutive mashings at 7 to 9 hour intervals
Yield:
5,104 British proof gallons or 6 i/io gal. per cwt.
SMALL LOWLAND POT STILL DISTILLERY ALL MALT
Batch :
1,000 bushels of malt
Wash:
20,900 gallons
Yield:
1,979 British proof gallons or 6.16 gallons per cwt. (with a high
class malt, skilfully manipulated, yield should be J to 7% gallons
per cwt.)
HIGHLAND POT STILL DISTILLERY ALL MALT
Equipment :
i wash still, 8,500 gallons capacity
i low wines still, 4,500 gallons capacity
Batch:
i, 800 bushels of malt 659 cwt.
n 4 WHISKEY MANUFACTURE
Wash:
37,730 gallons
4 successive mashings at 7 hour intervals
Yield:
4,370 British proof gallons or 6% gallons per cwt.
PATENT STILL DISTILLERY
Batch:
6,080 bushels of corn and malt 3,052 cwt.
(5,168 bushels of corn)
( 912 bushels of malt)
Wash:
216,500 gallons
Yield:
16,542 gallons of British proof spirit or 5.4 gallons per cwt.
Reduction in bulk, in one continuous operation, from 216,500 gallons
of wash to 9,930 gallons of spirit, or of 100 gallons of wash to 4.5 gallons
of spirit. The wash had an average spirit value of 7.8% of proof spirit
and the spirit produced an average spirit value of 165.2% or 65.2% o.p.
The relative quantities of spirit and feints in the collected distillates were
in the ratio of IOO proof gallons of spirit to 2.7 proof gallons of feints
(16,409.9 actual to 444.6 actual). In bulk, the ratio was 100 gallons
of spirit to 5.7 gallons of feints.
PATENT STILL DISTILLERY
Batch:
10,500 bushels of corn and malt 5,089 cwt.
(3,000 bushels of malt)
(7,500 bushels of corn)
Wash:
500,000 gallons wort
50,000 gallons yeast washings
Yield:
31,068.1 proof gallons or 6.1 proof gallons per cwt.
Rate of distillation:
2 Coffey stills operating 32 hours; rate per hour 17,187 gallons
Reduction in bulk in one continuous distillation was 550,000 gallons
(original wort, with yeast pressings, etc., recovered) reduced to 18,615
AMERICAN WHISKEY 115
gallons of spirit and feints, or in the ratio of 100 wash to 3.38 spirit and
feints. The wash had an average spirit value of 6.3 per cent proof spirit,
and the spirit and feints one of 166.9 P er cent proof (83.5 per cent by
volume).
The relative quantities of spirit and feints collected as distillates were
31,045.3 and 826.2 proof gallons; or in a ratio of 100 spirit to 2.6 feints.
The ratio of bulk was 100 spirit to 2.9 feints.
In considering yield figures it should always be borne in mind
that yield does not wholly depend on efficiency of distillation.
The quality of grain varies from year to year and though the dis-
tiller may pay more for his grain in one particular year it is quite
possible that the yield per cwt. will be less than in the preceding
year. This reduced yield is due to inferior grain and the rise
in prices to economic factors.
American Whiskey. General Statement. While the prac-
tice of whiskey manufacture in the United States varies quite
definitely from British practice, it is also divided within itself into
two general schemes. The divergences from British practice are
mainly in the method of preparing the grain before the actual
mashing (saccharification of the starch) ; in the general custom
of fermenting the whole mash rather than filtered wort; and in
the almost universal employment of patent stills. Within itself
American whiskey making may be classified as small scale and
large scale. There are definite differences of procedure and not
merely size of operation which distinguish the two groups.
Preparation of Wort. Small Scale. Not only is starch a
highly resistant material, but in cereal grains it is present in such
highly compressed masses that some variety of treatment is neces-
sary to loosen and spread it thinner before it is possible to convert
it to sugars with any degree of efficiency. In the British Isles this
object is accomplished either by subjecting the entire batch of
grain to the malting process or else by the use of one or another
modification of the acid conversion process. In the United States,
where mixed mash whiskey is made, the starch is "opened up" or
"pastified" by boiling with water, with or without the addition
of a small portion of malt. In "small scale" operation this cook-
ing is done at atmospheric pressure. The grain is ground to grist,
n6 WHISKEY MANUFACTURE
a portion of dry or green malt grist is added, hot water is poured
on in the ratio of 20 gallons per 56 Ib. bushel of grist, and heat
(steam) and agitation applied until the starch is "pastified."
While the primary object of the process is "pastification," the
addition of malt undoubtedly causes a slight amount of saccharifi-
cation to occur simultaneously. It is usual to start the cooking at
about 140 F. Live steam is then run into the open tank until
the batch boils. Boiling continues for about one hour and then
the batch is cooled to about 150 F. and the mashing commenced
by the addition of a suitable quantity of malt. Generally, in a
small distillery of this character, an open tank equipped with
agitator, live steam, and cooling coils is employed for the starch
pastification and the mashing is carried in the same vessel. Usu-
ally the malt, when introduced into the mashing vat, is at a tem-
perature of 1 25- 1 30 F. so that the batch after mixing will
have a temperature of about 140 F. The mash is held at this
temperature for a half hour or so and then warmed to about
150 F. After being held at this temperature for about one and
a half hours it is cooled to about 66 F. in the summer or 72 F.
in the winter.
Fermentation. The batch is then ready to commence the fer-
mentation. While it is possible to commence fermentation at a
somewhat higher temperature than those stated, it is also dan-
gerous as the reaction may overheat beyond control.
It has been suggested that the process just outlined may be
modified in the interest of malt economy, as follows: The mixed
mash is started at 135 F. and after thorough agitation, most of
the wort is drained off and stored temporarily. In the while, the
wet grain is again raised to boiling temperature and boiled for a
short time. Cold liquor is then added to reduce the temperature
to 140 F. and the stored wort pumped back and thoroughly
mixed with the balance of the mash. The subsequent procedure
is as above. This modified process was designed to permit a sec-
ond pastification of such starch as was uncooked in the first opera-
tion and provides no advantage if the first cooking was sufficiently
thorough.
AMERICAN WHISKEY 117
Distillation. Practically all American whiskey is distilled in
patent stills by the process described in detail for large scale
distillation.
LARGE SCALE OPERATION
The manufacture of whiskey on a large scale in the United
States represents the application to this process of all the im-
provements in efficiency and economy of time and materials made
available by modern Chemical Engineering knowledge. A dis-
tillery includes units for milling; yeast production; whiskey,
spirits and gin manufacture; recovery of secondary constituents;
blending; and reduction and recovery of slop. A diagrammatic
layout is shown as a whole in Figure 26 and the separate parts
in Figures 27-31.
Milling. The first operation at the distillery is the prepara-
tion of the grain and malt. These are elevated to hoppers and
passed over magnetic separators to remove tramp iron, etc.,
which might injure the crushers. The cereals are then fed to
grinders of the type commonly used for flour milling, and re-
duced to meal. The separate meals are then elevated to receivers
and hoppers by means of air conveyors, and fed to their respective
storage bins.
Cooking. Starch is completely pastified by cooking under
pressure. In order to maintain semi-continuous operation this is
accomplished in three cookers used cyclically at intervals of an
hour. That is, cooking of each distinct batch consumes three
hours, but each hour another cooker in rotation has completed
its batch and commences with a fresh one. A scheme of this
operation is shown in Figure 32, p. 125.
The charge is usually made up on the proportion of 15-20
gallons of water at 100 F. per bushel of grist. In the mash tun
more water or "slop-back" is added until the ratio is about 40
gallons per bushel. It will be noted that economy of steam is ob-
tained by using the high pressure steam from one cooker to pre-
heat another. Similarly, the use of a barometric condenser serves
to economize on cooling water. When the charge is properly
n8
WHISKEY MANUFACTURE
RECEIVER
EXHAUSTER
CENTRIFUGAL
SEPARATOR
GRAIN STORAGE MILLING
Fie. 37. (Courtesy E. B. Badger & Sons Co.)
AMERICAN WHISKEY
119
MASHING YEASTING & FERMENTING
FIG. 2$. (Courtesy of E. B. Badger & Sons Co.)
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WHISKEY MANUFACTURE
, WHISKEY DISTILLATION
FIG. 29. (Courtesy E. B. Badger & Sons Co.)
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WHISKEY MANUFACTURE
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AMERICAN WHISKEY
123
MASH RECOVERY
FIG. 32. (Courtesy E. B. Badger & Sons Co.)
I2 4
WHISKEY MANUFACTURE
TIME SCALE
COOKER No.
i
2
3
Charge with grist and
Steam bled to No. I
Cold malt mash
Hour
water.
cooker.
added. Kept at
i45F. for ist 1 5 min.
Steam bled from No. 2
1 50 F. for 2nd 1 5 min.
cooker.
Live steam at 50 Ib.
Steam bled to baro-
Discharge to mash
pressure.
metric condenser. Kept.
tun.
boiling until cooled to
150 F. 22" vacuum.
Steam bled to No. 3
Cold malt mash
Charge with grist
i
Hour
cooker.
added. Kept at
and water.
145 F. for ist 15 min.
i5oF. for 2nd 15 min.
Steam bled from
No. i Cooker.
Steam bled to baro-
Discharge to mash
Live steam at 50 Ib.
metric condenser. Kept
tun.
pressure.
boiling until cooled to
i5oF. 11" vacuum.
Cold malt mash
Charge with grist and
Steam bled to No. 2
i
Hour
added. Kept at
water.
cooker.
145 F. for ist 15 min.
i5oF. for 2nd 15 min.
Steam bled to No. 3
cooker.
Discharge to mash
Live steam at 50 Ib.
Steam bled to baro-
tun.
pressure.
metric condenser.
Kept boiling until
cooled to 150 F. 22"
vacuum.
3
Hour
Recharge as at o hour.
Steam bled to No. i
Cold malt mash
cooker.
added. Kept at
145 F. for ist 15 min.
1 50 F. for 2nd 1 5 min.
FIGURE 33. 3-Hour Cooking Cycle in Large American Distillery.
AMERICAN WHISKEY 125
cooked it has the consistency of a thick soup and all of its starch
is quickly accessible to the diastatic action of the malt.
Mashing. The mash is then pumped to the mash tun and
water, or liquor from the spent slop tank if a sour mash is de-
sired, is introduced in sufficient quantity to make the ratio of the
total mash 40 gallons of liquid per bushel of grain and the batch
is agitated while the mashing operation proceeds under tempera-
tures and conditions approximately equivalent to those previously
described under "mashing processes/'
Fermentation. At the conclusion of the mashing operation
the whole contents of the tun are pumped, usually to an inclosed
cooler. In this type of cooler the mash is forced through a double
pipe system and is cooled by a counter current of water down
to 70 to 80 F. This is a radical departure from Scotch and
Irish practice in which only the wort is used for fermentation.
A small portion of the mash is bypassed to an auxiliary mash tank
which forms part of the yeast propagating system. The main
mash Is pumped from the coolers to the fermentation tanks and
a certain amount of yeast is added from the yeast growing system.
Fermentation soon commences and the temperature is controlled
by means of cooling coils. It will be observed from the diagrams
that the heating and cooling operations are effected by means of
coils within the tanks. After completion of the fermentation
the "beer" is pumped to the "beer well," a tank which is fitted
with an agitating device thoroughly to stir the beer and prevent
any settling.
Distillation. At this stage of the process there are several
interesting variations from Scotch and Irish methods of distilla-
tion. Note, on the diagrams, that by means of a bypass system
the beer well may be connected to either the whiskey or spirit
stills; these are both termed beer columns, although they are
really distinct kinds of stills.
Various economies and several different methods of operations
are effected by the aid of an elaborate piping system. Both the
whiskey and the spirit stills are equipped with heat exchanging
apparatus so that the still vapors passing through the heat ex-
126 WHISKEY MANUFACTURE
changers give up their latent heat to the beer as it is pumped
through the apparatus on its way to the stills. In other words,
pre-heating of the beer is effected by means of the latent heat of
the still vapors.
The whiskey still consists of a column equipped in the head
with two rectifying plates and one washing- plate. In this very
efficient arrangement ascending alcoholic vapors are rectified so
that their alcoholic content is increased from approximately
6 per cent to 72 per cent. This effects in one continuous opera-
tion, and more efficiently, the same doubling of concentration
achieved by the European pot still equipped with a doubler as
shown in Figure 15 in Chapter VIIL The rectified vapors then
pass through the heat exchanger and then into the condensing
system. As they emerge from the condensing system they are
tested for strength and content of secondary products.
Another advance over European practice at this point is the
fact that by means of the control system it is possible either to
pass the condensates back to the column for reflux purposes or to
withdraw them to a test box. By these means, a whiskey of
almost any desired secondary product content can be produced at
the will of the distiller, depending on the rate of reflux em-
ployed. The distillate when diluted with distilled water to about
100 proof (50% by volume) is ready to barrel as whiskey.
The spirit still is a typical continuous alcohol rectifying still
equipped with heat exchanging device for pre-heating the beer
fed from the beer well and with various rectifying units for re-
moving both lower and higher boiling impurities, especially alde-
hydes and higher alcohols. By means of control and concentra-
tion devices a practically pure, 96 per cent spirit can be produced.
These spirit units recover more than 98 per cent of all the
alcohol present in the beer and produce 90 per cent of this alcohol
as high grade U. S. P. spirits and the remainder as heads and
a washed fusel oil. Such a unit will use about 40 pounds of steam
per gallon of alcohol produced. The largest of these units now
in use produces 18,000 gallons of spirits per day of 24 hours.
Figure 31 shows a mash recovery system. Here the spent
AMERICAN WHISKEY 127
still liquor, or slop, is received, agitated, and passed over a
screen to filter out the solids. The solids are fed to a press to
squeeze out residual moisture. The liquor is discharged to the
spent slop tank, while the damp solids are then fed to a rotary
drier of standard design, which drives off any remaining moisture.
A blower delivers the dried solids to a receiver fitted with a hop-
per which feeds the material to a packaging device. Recovery
of solids is approximately 12 to 15 pounds per bushel.
Unless legislation or peculiar local conditions require total
evaporation the thin slop is discharged to the sewer or part is
returned if process calls for "slopping back."
Aging. Whiskey as first produced by any of the processes
described is raw and unpleasant to the taste and disagreeable in
odor. It has been known for very many years that by storage for
a period of time, changes in the odor and taste are produced
which result finally in the ripe smoothness of taste and pleasant
odor associated with good whiskey. Despite much work the
whole chemical nature of these changes is still incompletely
known. As the late William Howard Taft concluded from an
investigation made during his presidency: "It was supposed for
a long time that by the aging of straight whiskey in the charred
wood a chemical change took place which rid the liquor of fusel
oil and this destroyed the unpleasant taste and odor. It now
appears by chemical analysis that this is untrue that the effect
of the aging is only to dissipate the odor and modify the raw,
unpleasant flavor, but to leave the fusel oil still in the straight
whiskey."
Actually, comparative analysis of old and new whiskey shows
a somewhat greater content of secondary constituents in the old
matured whiskies, especially in the relative amounts of volatile
acids and aldehydes. The esters also increase, but to a lesser
extent, while the furfural and higher alcohol contents remain
practically unaltered. Of course, whiskey stored in wooden bar-
rels increases in proof due to a relatively more rapid diffusion
of water through the pores of the wood. In obtaining the
analytical results noted above, this change is compensated by
128 WHISKEY MANUFACTURE
calculation to a uniform base alcoholic strength. The solids con-
tent and color of the whiskey increase markedly on aging due
to the extraction of tannin, resins and other materials from the
wood. The density of color is directly proportional to the solids
content in an aged whiskey.
Aging practices differ somewhat. British custom is to store
the whiskey in uncharred oak barrels while American whiskies,
both Rye and Bourbon, are stored in charred barrels. The color
and solids of whiskey aged in uncharred packages are much
smaller in amount and more water soluble than those of whiskey
stored in charred packages. The charring also results in a "bead"
of oilier consistency and greater permanence than the uncharred
barrel imparts.
Rye whiskies are stored in heated warehouses, while Bourbons
are matured in unheated buildings. As a result the former are
stronger in color than the latter. In general, whiskey does not
improve at all after about ten years of storage, although there
still continue slight changes in composition; nor is there any very
marked improvement in desirable character after the first four to
six years of storage. The high price of very old whiskies is
largely to compensate for evaporation losses which become very
marked, and the carrying charges on investment tied up for long
terms of years. Storing has its limitations. A fifteen year old
whiskey maybe a bad whiskey because, as President Taft pointed
out, its fusel oil content has increased too much. There are whis-
kies only two years old far better in flavor than hoary distillates
that have been kept in barrels for two decades.
Artificial Aging. The chemist distinguishes between aging
and maturation; that is, between the mere passage of time and
the effects thereby produced. If the latter can be duplicated
within a short period, the results, from the chemist's and from an
economic point of view are much preferable. Hence much study
has been given to the subject of the artificial aging of spirits.
Many of the more scientific suggestions are admirably summar-
ized by Snell and Fain in an article which appeared in Ind. &
Eng. Chem. News Ed. XII, 7, p. 120. They state:
AMERICAN WHISKEY 129
The Legalization of Traffic in spirituous liquors in this country has
created a situation which puts a premium on naturally aged alcoholic
beverages. To satisfy the demand for liquor at a popular price, the avail-
able stocks on hand have to be increased either by blending or accelerated
aging.
During the aging process the constituents of alcoholic spirits undergo
chemical change. A study of the changes taking place in whisky stored
in wood over a period of eight years revealed (5) important relations
between the acid, ester, color, and solid contents of a properly aged whisky
which will differentiate it from artificial mixtures and from young spirits.
High color, high solid content, and high alcohol concentration are gen-
erally accompanied by high acid and ester content; low color and solid
content go with a small amount of acids and esters. In the aging process
the acids are at first formed more rapidly than the esters. Later the esters
form more rapidly so that by the end of the fourth year they are present
in the same amounts. The equilibrium reached at this period is main-
tained. The amounts of higher alcohols increase in the matured whisky
only in proportion to the alcohol concentration. The oily appearance of
a matured whisky is due to material extracted from the charred container ;
this appearance is almost lacking in whiskies aged in uncharred wood.
The improvement in flavor of whiskies in charred containers after the
fourth year is due largely to concentration. The higher content of solids,
acids, esters, etc., of rye over Bourbon whiskies is explained by the fact
that heated warehouses were used for maturing rye whiskies and unheated
warehouses for maturing Bourbon.
The aging of brandy, similar to that of whisky, takes place in oak
casks. The conjoint action of the oxygen of the atmosphere and the
resins, gums, and tannins extracted from the wood are responsible for the
improvement of the liquor. These compounds, being capable of easy oxi-
dation, pass through a series of reactions. Aromatic compounds particu-
larly agreeable in taste and odor are formed.
Aging of spirits involves oxidation. It is this reaction which one
attempts to hasten by the processes devised for accelerated aging. Methods
for aging spirits artificially fall into four main classes as follows : ( I )
treatment with air, oxygen, or ozone; (2) exposure to actinic rays; (3)
electrolytic treatment; and (4) use of catalysts. Combinations of these
methods are likewise employed.
TREATMENT WITH GASEOUS OXIDANTS
A recent example of the first type provides for treatment (77) of the
liquor with oxygen while exposed on large wooden surfaces which have
130 WHISKEY MANUFACTURE
been impregnated with a solution obtained by extracting seaweed ash.
Brandy (28) is artificially aged by bringing it into contact with activated
charcoal which may first be treated with a current of air or oxygen.
Oxidation may be accelerated by the use of compressed air (6). The
liquid to be treated is run into a tank which can stand a pressure of
several atmospheres. Compressed air enters from the bottom of the tank.
The length of time required for treating by this process depends mainly
on the pressure of the air, the nature of the liquid, and the extent of aging
desired. In a special apparatus (21) for this purpose, the liquid is sprayed
or atomized in a chamber containing air under pressure by delivering from
two oppositely disposed nozzles with a double cone between. Intimate
mixture is obtained. As a modification of methods for treatment with
oxygen in high concentration, beverages such as brandy, cognac, and liqueurs
(13} are cooled to a temperature below 18 C., saturated repeatedly
with air while at this temperature, and afterward stored in a warm room
until the acids combine with the alcohols forming esters. According to a
Canadian process (26) oxygenating gas is bubbled through new spirits
in a vat. The gas, after passing through the liquid, rises through a mass
of shavings or cuttings of charred or desiccated wood (preferably oak) over
which a counterflow of the spirits is maintained by withdrawing liquid
from the bottom of the vat and discharging it into or over the wood.
Alcoholic beverages, such as whisky, cognac, etc., are also treated with
air (2) which has been subjected to a high-tension electric arc. This air
contains oxides of nitrogen. The claim is made that the flavor is improved.
Aging has been accomplished (4) by bringing the liquid in contact with
bodies such as oak chips or shavings which have been treated with ozonized
air or oxygen. This prevents local excess concentration of the ozone.
Apparatus has been developed (/) for the production of ozone for use
in the accelerated aging of liquors. Sizes up to 300 kw. with capacities
up to 10 to 12 kg. of ozone per hour are available. Concentrations of 2
to 4 grams of ozone per cubic meter can be obtained in air or oxygen,
with an energy consumption of 25 to 35 kw-hr. per kg. of ozone. Treat-
ment of liquor with ozone gives a mellowing effect in a short time which
can be obtained otherwise only after months or years of storage. Analysis
shows a decreased aldehyde content and an increased ester content. A
suitable ozonizer for liquor treatment is a special 50-watt size with a
capacity of 100 liters per hour.
USE OF ACTINIC RAYS
For artificial aging of wines and liquors by the action of ultra-violet
light (7), a vapor electric arc having a quartz container is used. The
AMERICAN WHISKEY 131
liquor is passed over this lamp in a thin film. In several processes actinic
rays are used in combination with oxygen or an oxidizing agent.
One process (16) subjects them to light from a neon lamp ranging
from yellow to orange in color, in the presence of oxygen. Another (20)
subjects them to ultra-violet rays after addition of a small amount of
hydrogen peroxide, inorganic and organic peroxide, or ozonide.
As another variation (ig) wine, cognac, etc., are aged and improved
by pretreating with ultra-violet light the water used in their preparation.
The water may also be aerated or treated with oxidizing agents. The
product after addition of the water is sometimes irradiated.
ELECTROLYTIC TREATMENT
Beverages are artificially aged by an electrolytic treatment (14) pro-
ducing hydrogen and oxygen in the liquid. The electrodes and the dia-
phragm between them are impregnated with insoluble inorganic salts or
oxides capable of producing oxidation and reduction effects in the presence
of the oxygen and hydrogen produced.
In aging and maturing alcoholic liquors by electrolysis (10, //), a
depolarizing cathode and a current of low intensity are used. The cathode
is formed of a carbon electrode surrounded by manganese dioxide and
carbon contained in a porous pot. The anode is formed of a nonoxidizable
metal such as gold. The electrolysis is effected in the presence of the
substances which the spirits will extract from oak wood. For this purpose
the spirits are allowed to remain for some time before treatment in oak
casks. Sometimes oak shavings are added to the spirits during treatment.
The electrolysis will, owing to cataphoresis, assist in the extraction. The
electrolysis may be effected in oak casks between anodes on the outside of
the cask and a cathode inserted through the bunghole. Pads of moist linen
or cotton are placed between the anode and the surface of the cask. The
vats and casks are supported on insulators which may be bowls containing
a liquid such as vaseline oil. The passage of current is maintained con-
tinuously for eight to ten days, according to the conditions adapted for
each application.
Apparatus (8) for treating liquids such as wines, spirits, etc., with
electrical currents of high voltage and low amperage, consists of two point-
and-disk separators placed oppositely in parallel circuits connected to the
terminals of a transformer, so that one alternation of the transformer cur-
rent will pass through one circuit and the other alternation through the
other. Barrels containing the liquid to be treated are inserted in each
circuit. By the use of this method there is no heating of the liquid, and
loss by volatilization of the aromatic compounds contained in the liquor
132 WHISKEY MANUFACTURE
is minimized. Another process (p) ages wine, cognac, and arrack by
passing a high-tension electric discharge through them. The combination
of the electrolytic treatment with the use of air, oxygen, or ozone has
likewise proved effective.
Suitable apparatus (23, 24, 25) combines treating liquor in barrels with
a gas, such as air, oxygen, or ozone, and the use of an electric current to
accelerate aging. An electrode is inserted through the bunghole of the
liquor container, and the liquid either alone or together with a fine wire
of high resistance connecting the electrodes serves as conductor. Heating
of the liquid occurs in either case.
An ingenious process (18) includes saturation of the liquid with oxy-
gen, followed by the transformation of this oxygen into ozone by means
of discharges of electricity through the liquid. The oxygen is introduced
into the liquid under pressure and the electricity is discharged at short
intervals through the liquid. Impurities from distillation are oxidized and
the flavor is improved.
USE OF CATALYSTS
Artificial aging of spirits is aided by the use of catalysts. The vapors
may be passed over finely dispersed metal oxides such as those of copper,
nickel, and titanium (27) at 150 to 180 C.
Suitable catalysts for oxidation (22) are oxides of cobalt, cerium,
vanadium, and uranium. Catalysts for ester formation are oxides of lead,
molybdenum, silicon, uranium, and cerium. The best flavors are produced
by the use of oxides of lead, copper, nickel, molybdenum, cobalt, titanium,
and silicon.
Charcoal and charred sawdust have likewise been found to catalyze
the maturing of spirits. The rising vapors, inside or outside the cask,
may contact catalytically acting charred sawdust or charcoal (29) with-
out the catalyst, however, coming in contact with the liquid. Other cata-
lysts may be employed in this way, alone or together with the charcoal or
charred sawdust.
A similar method ( j) for maturing potable alcoholic liquors is to mix
the vapors from a pot still with heated air, subdivide the mixture into
narrow streams, and pass this through a narrow conduit heated to about
1 50 C. The streams are joined and the treated vapors condensed. The
heated metal walls are supposed to act catalytically to produce the desired
result.
MISCELLANEOUS PROCESSES
Spirits are also aged (15) by separating alcohol and water, and re-
moving the fusel oil from the concentrated extract of oils, etc., by treat-
AMERICAN WHISKEY 133
ment with petroleum ether. The concentrated extracts are subjected to
accelerated aging by one of the methods described above, and again mixed
with alcohol and water free from fusel oil.
According to another process ( 12) an extract prepared from oak wood,
such as is used in making the usual storage vats, is added. The wood,
which may be the heart of the larger branches of the trees or the waste
obtained in making casks, is disintegrated and submitted to two successive
extractions with aqueous alcohol and a final extraction with water. The
alcoholic extracts are distilled in vacua at a low temperature, the residue
is added to the aqueous extract, and the mixture is evaporated in vacuo to
obtain the extract in the form of a dry solid.
The old principle of acceleration of a chemical reaction by heat is
applied to wines and spirits by storing them in closed vessels and agitating
(30) for some months at 43 C. A rocking, effected by oscillating a
platform on which the cask rests, rather than by a tremulous vibration, gives
the desired results.
The lines of attack on the problem are sound and can be expected to
give results when properly applied. Details as to application vary in dif-
ferent processes. Some are in commercial use today in our newest large
industry.
LITERATURE CITED
(1) Becker, J., Chem. Fabrik, 1929, 49.
(2) Brabender Elektromaschinen G. m. b. H., German Patent 500,-
708 (1928).
(3) Carroll, J. E., U. S. Patent 968,832 (1910).
(4) Coffre, R., British Patent 340,647 (1928).
(5) Crampton, C. A., and Tolman, L. M., /. Am. Chem. Soc.j 30,
98 (1908).
(6) Deriques, J. L., Z. Spiritusind., 31, 141 (1908).
(7) Henri, V., Helbronner A., and von Recklinghausen, M., U. S.
Patent 1,130,400 (1910).
(8) Henry, C., British Patent 17,400 (1914)-
(9) Hirschmann, W. A., German Patent 199,265 (1907).
(10) Jarraud, A, British Patent 141,687 (1920).
(n) Jarraud, A., German Patent 239,3OO (1910).
(12) Jarraud, A., and Roussel, J., British Patent 148,829 (1920).
(13) Monti, E., U. S. Patent 1,108,777 (1905)-
(14) Nottelli, L. E., French Patent 711,300 (1931)-
(15) Philipsky, J. H., German Patent 549,524 (1929).
(16) Ibid., 557,8o6 (1930).
(17) Ibid., 572,351 (i932).
134 WHISKEY MANUFACTURE
(18) Plotti, A., Progres agr. vit., 24, 674 (1908).
(19) Reinisch, E., Austrian Patent 112,976 (1928).
(20) .Ibid., 115,902 (1929)-
(21) Saint-Martin, W., German Patent 237,280 (1910).
(22) Sandor, Z, de, Mezogazdasdgi Kutatdsok, 4, 468 (1931).
(23) Seitz, J., U. S. Patent 961,167 (1908).
(24) Ibid., 967,574 (1908).
(25) Ibid., 967,575 (1909).
(26) Sunderman, F. R., and Gaut, R. E., Canadian Patent 303,644
(1930).
(27) Toth, G., Magyar Chem. Folyoirat, 38, 129 (1932).
(28) Verdeaux, F., French Patent 716,829 (1931).
(29) Verein der Spiritus Fabrikanten, German Patent 291,349
(1915).
(30) Vianna, J. da V., British Patent 23, 548 (1913).
Dosing. It is also claimed and has probably been practiced
that the addition of small proportions of the materials listed
below either singly, or in combination, will improve the flavor and
appearance of whiskey.
Acetic Acid
Allspice
Almond shell extract
* Beechwood creosote
Caramel
Caraway seed
Cedar wood extract
Cherries, dried
Cherry juice
Cinnamon
Cloves
Glycerin
Glycerite of tannin
Oak extract
Peach juice
Peaches, dried
Plum juice
Plums, dried
Prune juice
* Beechwood creosote is said to have been the material used during prohibition
for imparting the smoky taste to bootleg Scotch whiskey.
AMERICAN WHISKEY 135
Prunes, dried
Sherry wine
Spirit of nitrous ether
Tannic acid
Vanilla
Walnut shell extract
Catechu tincture
Coumarin
Kino tincture
Orris root
Pekoe tea
One of the less scientific methods for accelerating the matura-
tion of whiskey was aging for comparatively short periods in
old sherry wine casks. This method was claimed not only to be
very effective but also is probably the least objectionable. As a
variation the casks could be subjected, before filling with whiskey,
to a forced seasoning. The process consisted of placing the casks
bung down and drying them thoroughly by forcing a current of
warm air through the bunghole. Then enough wine to wet all
the inner surface was poured into the cask, the cask revolved to
coat all the wood and the wood impregnated by forcing in warm
air under pressure.
Blending. On account of the inherent variability of a prod-
uct made in relatively small batches like pot still whiskey; and
the natural fluctuations in the qualities of the raw materials avail-
able for patent still whiskey, the practice of blending whiskey of
different distillations and different years arose early in the life of
the industry, to enable the distiller to market a more uniform
product. Later, the custom extended to the blending of the
products of different distilleries and of distillates from both pot
and patent stills. Still later, and in the United States possibly
even more after the repeal of prohibition, the practice of spread-
ing the flavor of an old whiskey over three to five times as much
diluted u silent spirits" was exceedingly common.
In Great Britain the business of blending has assumed great
importance within the industry as can be shown by reference to
the Directory of Whiskey Brands and Blends which lists 3428
136 WHISKEY MANUFACTURE
Scotch, 487 Irish, and 128 Scotch and Irish blends founded upon
the output of 122 Scotch and Irish distilleries.
The practice has both good and bad features. For example,
the blender can take the distillers' output and by skillful blending
produce a product of uniform characteristics year after year with
little variation. Again, qualities desired of whiskey vary accord-
ing to the locality. For example, Scotland, Canada and Scandi-
navian countries favor stronger whiskies than those drunk in
England, France, Belgium, Holland, Australia and India. It is
hard to say what the United States now favors, probably a strong
whiskey. The blender can meet these geographical differences in
taste by skillful blending. On the other hand, cheap and inferior
blends have often been foisted upon the public under misleading
names.
Blending formulae are secret, and the practice as carried on
by some of the oldest and most conservative blenders approaches
an art. At its crudest it consists of pouring the various whiskies
into a blending tank according to formula, dosing, coloring and
stirring the mixture and then allowing it to rest for 24 hours.
The blend is aged in a cask for a short time and then bottled.
This gives a raw whiskey, imperfectly blended, and fit only
for a cheap trade. A good blender proceeds more as follows:
First, he selects various fine malt whiskies. He blends these care-
fully, marrying one whiskey with another every three months
until the desired body and flavor are obtained, and then ages
them in an uncharred oak cask for about two years. When he
deems the blending and aging to be complete, he mixes the prod-
uct with patent still spirit and Lowland or equivalent malt, stirs
them up and allows them to age again in an uncharred oak cask
for a year or more.
Scotch pot distillers have admitted the necessity of blending
both pot and patent still products, except when the pot still spirit
has matured for a considerable number of years in wood, in which
case they consider it unnecessary. They claim that it is the pot
still product which imparts character to the blend and that con-
sequently it must always be employed in preponderating propor-
AMERICAN WHISKEY 137
tion in the blend if the reputation, which the best classes of Scotch
whiskey have gained, is to be maintained.
The production of cheap and palatable Scotch whiskies in-
volves a different set of considerations. It is necessary for pot
still spirits to mature in wood in order that they should acquire
a pleasant flavor. Patent still whiskies, on the other hand,
although they are improved by aging in wood, change to a less
extent and mature much more quickly. It is stated that by
blending immature pot still with patent still whiskey the pungent,
unpleasant taste of the former is attenuated or toned down and
that the mixture then becomes u a palatable and not unwholesome
spirit." Such a mixture, if stored in wood, would mature in a
shorter time than would the pot still whiskey alone.
The proportion of pot still to patent still whiskey in these
cheap blends is varied chiefly in accordance with the price at
which they are planned to sell. The cheapest blends may con-
tain as little as 10 per cent of the former and even less.
Irish distillers contend that it is unnecessary to blend aged
Irish pot still whiskey with patent still spirits, but admit that such
blends are made for the cheaper trades. By British law the age
of the whiskey in a bottle is determined by the age of the young-
est whiskey in it, irrespective of the amount of that whiskey.
Let us suppose that there are fifteen whiskies in a bottle, aver-
aging fourteen years and making up 99 per cent of the contents,
while i per cent is a whiskey aged five years. The legal de-
clarable age of that whiskey is five years. White lies have been
told on labels bearing such inscriptions as "Whiskey in this bottle
is fifteen years old." It is true that there may be whiskey in that
bottle aged fifteen years, but the real story is not there.
Post repeal American blending practice is still, at the time of
this writing, in a chaotic state. The same general principles of
desirable and undesirable blending are applicable as in British
practice. The details of blending in this country as well as the
tremendously complicated system of combined federal and sep-
arate state legislation are in an almost continuous state of flux
so that there is little to gain by recording them. With the advent
138 WHISKEY MANUFACTURE
of repeal in this country, stocks of aged whiskey were much below
the anticipated demand. Hence, most such stocks were "blended"
or "cut" with very new whiskey or even with diluted alcohol and
other materials, colored with caramel, dosed with "prune juice 11
and "bead oil" and sold quickly. Very shortly the flood of
federal and state regulations appeared. These range from re-
quirements that a "blended whiskey" shall contain not less than
20 per cent of four year old "U. S. P. Whiskey" to requirements
similar to the British, that blended whiskey shall bear on its label
the age of the youngest whiskey it contains. The reader is re-
ferred to Chapter XIII on interpretation of analysis for further
details on this topic.
CHAPTER X
BRANDY, RUM, GIN
AND
OTHER DISTILLED LIQUORS
BRANDY
Brandy is the product prepared by distilling wine, wine lees
and/or grape pomace and often by blending the results of these
operations.
It is a yellowish-brown liquor of sweet, smooth ethereal
flavor and of fine bouquet. Alcoholic content is usually from 45
to 55 per cent by volume.
As first made it is normally colorless, and the familiar yellow-
ish-brown hue is obtained either naturally by aging in oak casks
or artificially by addition of a solution of caramel.
The fine flavor and bouquet result from the secondary con-
stituents of the brandy and are dependent upon a number of fac-
tors, principally raw materials, operating methods, aging, etc.
The secondary constituents consist of various esters (acetic,
butyric, oenanthic, valerianic), acetic acid, volatile oils, tannin,
fixed acid and coloring matter. Ethyl pelargonate (oenanthic
ester) and other volatile constituents are thought to be mainly
responsible for the flavor.
Because of the fine quality of its products France is com-
monly thought of as the home of brandy. However, other coun-
tries are also large producers: e.g., Spain, Egypt, South Africa,
Australia, Algeria, Germany and the United States (California).
Spanish and Algerian brandies are of very high quality. Egyptian
brandies are made from imported grapes (Asia Minor and
Southern Turkey) and have a strong flavor. They are not so
fine and compete with the cheaper brandies. Australian and
139
1 40 BRANDY, RUM, GIN
South African brandies are of fair quality. South African "dop"
brandy is an "eaux de vie de marc."
Brandies are produced in various parts of France. The best
are produced in the Cognac district which is located in the two
departments, Charente and Charente Inferieure. The region
is also divided, according to the fineness of the wine, into the
Grande (or fine) Champagne, the Petite Champagne, the Bor-
deries and the Bois. Next in order of commercial merit are
those made in the Armagnac, including the Marmande district.
Other parts of France in which brandies are produced are:
le Midi, Aude, Card, Herault and Pyrenees Orientales. Brandies
from these districts are commonly known as the "Trois-Six de
Montpellier."
Eau-de-vie is the French name for brandy. It is used there
in a rather broad sense and may embrace spirit distilled from
wine, cider, perry, marc, cherries, plums or other fruit and also to
mixtures of such spirits, or to a blend of any such eau-de-vie with
any "alcool d'industrie" which is a name for either grain or
beet alcohol. In view of this all-embracing nature of the term
it is customary for a Frenchman to qualify his order for an eau-
de-vie by specifying "un fine," or "fine champagne" or "un co-
gnac"
True brandies may be classified into the following grades :
First. Distilled from high quality light white wine not less
than a year old.
Second. Distilled from second grade wines or spoiled and
soured wines which have been specially treated before distilla-
tion.
Third. Distilled from grape pomace which may have been
refermented with sugar and water. The term "grape pomace 1 '
includes the skins, pulp and possibly the stems of the fruit. These
brandies are naturally of very inferior quality. They are known
as Marc Brandies or "eau de vie de marc" from the French term
for pomace. During prohibition a similar product was supplied
in the United States by bootleggers under the name "grappo."
Fourth. Certain incrustations are left on the sides and bot-
toms of fermentation tanks and aging barrels. They are called
BRANDY 141
u wine lees 11 and usually contain from 20-35% f potassium acid
tartrate (Cream of Tartar) and up to 20% calcium tartrate.
They also contain yeast cells, and protein and solid matter which
had settled out from the grape juice. By acidifying the lees with
sulphuric acid and distilling, a product of exceedingly strong
flavor and odor is obtained which is used to give character to
diluted silent spirits, and the product is marketed as brandy.
Distillation. In the Cognac district the brandy is made either
by the large distilleries or by the farmer himself right at the
vineyards. It receives very little rectification, when distilled, in
order to conserve the secondary constituents which produce the
bouquet and flavor.
For this reason, the simplest pot stills or slight modifications
thereof are generally used. The only usual modifications are
the pot still with "chauffe-vin" and the "a premier-jet" still. Ca-
pacity of the stills as a rule is about 150 to 200 gallons.
A "chauffe-vin" is a heat exchanging device for preheating the
wine before it reaches the still kettle. It consists of an arrange-
ment whereby the neck of the pot still passes through a wine con-
tainer so that the vapors, prior to condensation, give up part of
their heat to the wine in the tank. Sec Figs. 12, 13.
The "a premier jet" is a device for returning the distillate to
a heat exchanging attachment at the head of the still. By this
arrangement the newly rising still vapors give up part of their
heat to the first distillate which is thus vaporized. Some rectifi-
cation of the still vapors takes place. The a premier jet gives
some effect of continuous rectification as compared to discon-
tinuous operation with the ordinary pot still and the resulting
product is stronger but not of such fine quality. These brandies
are usually considered more suitable for liqueur manufacture
than for direct consumption.
In the simple pot still process, two distillations are used, which
may be compared with the process of whiskey making in the
Scotch pot still distilleries; the two distillates are respectively
termed "brouillis" and "bonne chauffe" the terms being directly
equivalent to the "low wines" and "spirits" of the whiskey dis-
tiller. The stills are worked very slowly and regularly, ten hours
142 BRANDY, RUM, GIN
are usually allowed to complete the distillation of a batch. The
quality of the resulting brandy, still depends to a great degree on
the judgment and skill of the operator.
In other districts where the wines have a strong, earthy flavor
somewhat more elaborate apparatus is used. The La Rochelle
district uses the Alembic des lies which is a pot still with rectify-
ing equipment. The Midi uses a continuous distilling column of
the kind in favor in this country, excepting that it is equipped
with a faucet or tap at each plate. This arrangement enables the
operator to distil at higher or lower strengths at will.
The wine used in the manufacture of Cognac contains from
6 to ii per cent of alcohol, or from 12 to 22 per cent of
proof spirit; the average strength is from 7^ to 8^2 per cent of
alcohol or from 15 to 17 per cent of proof spirit. The final dis-
tillate as run from the still is about 25% over proof or 60 to
65% in alcoholic content.
Aging. Following distillation the brandy is aged in oak
casks. Considerable care must be taken in the ripening process if
the distiller wishes to market a good product. Four or five years
at least are required to develop the right bouquet, flavor and mel-
lowness. The finest brandies are sometimes aged for twenty years
or even longer.
Before filling, the casks are thoroughly sterilized, either by
steaming, or by scalding with several changes of boiling water.
Following this, the cask is filled with white wine to dissolve any
objectionable coloring matters or substances which might affect
the flavor of the brandy and drained.
Blending. Aged brandies are very often blended, since they
may vary in characteristics according to source of raw materials,
district of production, and year of vintage. Blending has been
found necessary to produce a product of uniform characteristics
year after year. As in whiskey blending, cheapening may also
be a desideratum.
Formulae are, of course, secret and are based on the ex-
perience of the blender. They are generally varied each year, to
some extent, to compensate for the variation in characteristics of
the brandies available. The methods of procedure outlined under
RUM 143
Blending in Chapter IX on Whiskey apply, on the whole, to
brandy blending.
Many imitation brandies are on the market and it is very
doubtful how much of the brandy consumed is genuine. Imitation
brandies are made as a rule by cutting strongly flavored brandy
with diluted, rectified grain alcohol, coloring and sweetening with
caramel and cane-sugar syrup, adding small amounts of aromatic
substances, and dosing with either "lees oil" or an extract of oak
wood chips.
Various extracts are used to give to the brandy aged and
other characteristics. For example a wine distillate extract of
cedar wood chips, i to 10 (about 500 c.c. per 100 liters finished
product), gives wine and brandy a herb-like, typically aged char-
acter. A wine distillate extract of bitter almond shells (100 to
300 c.c. per 100 liters finished product) gives in addition to the
herb-like flavor a pleasant aroma resembling vanilla. The same
quantities of extract of either dried, green walnut shells or dried,
stoned plums round out the flavor nicely. Orris root, coumarin,
cinnamon, Pekoe tea and vanilla are also used although the wine
laws of some countries prohibit their employment. Many of the
products listed as dosing agents in Chapter IX on Whiskey have
also been used.
British Brandy. This is a compounded spirit prepared by
re-distilling duty paid grain alcohol with flavoring ingredients or
by adding flavoring materials to such spirits. The flavoring ma-
terials used in any one case are a trade secret, but in general are
to be found in the lists mentioned.
Hamburg Brandy. This is an imitation grape brandy made
by adding flavoring to potato or beet alcohol.
RUM
Rum is a spiritous beverage prepared by fermentation, dis-
tillation and aging, from molasses and the scum and foam which
form on the top of sugar cane juice when it is boiled. Fresh sugar
cane juice may also be used when the cost of sugar production
makes it profitable. High quality rums are made from mashes
containing comparatively small amounts of skimmings (scum).
144 BRANDY, RUM, GIN
So-called "Nigger rum" is made from mashes consisting princi-
pally of the skimmings and other waste products of the defeca-
tors of sugar cane factories.
Rum is a yellowish-brown liquor of fine bouquet and sweet,
smooth, alcoholic taste and flavor which cannot be successfully
imitated artificially. The alcohol content of the genuine product
should not be less than 78 per cent by volume. "Nigger rum" has
a raw, sour, burnt taste and flavor.
When first made, rum is normally colorless and the familiar
yellowish hue is obtained by aging in casks. If an exceptionally
dark color is required it is dosed with caramel.
Because of the fine quality of its products Jamaica is com-
monly thought of as the home of rum. However, rum is pro-
duced in all countries where sugar cane is abundantly grown; e.g.,
British Guiana, West Indies, Brazil, southern United States,
Madagascar and the East Indies.
Jamaica rum is graded into three classes, namely: I. "local
trade" quality for home consumption, 2. "home trade" quality for
consumption in the British Isles, and 3. "export trade" quality for
export. Local trade rum, the lowest quality, is distilled with
particular emphasis on its alcoholic strength to the neglect of the
other substances, chiefly esters, from which the flavor is derived.
The flavor of this grade is, therefore, decidedly inferior.
The "home trade" quality constitutes the bulk of the ex-
ported rum. It has a full flavor, and chemically is characterized
by a higher proportion of esters of higher fatty acids. It is gen-
erally accepted that these acids result from bacterial decomposi-
tion of the dead yeasts found in the distilling materials. As
compared with "local trade" goods the "home trade" have a
fuller and more fruity aroma and a marked spicy residual flavor
is noted on dilution. Sometimes, even, an excess of the higher
alcohols and esters which produce this result will also cause an
objectionable cloudiness on dilution with water. On occasion
"home trade" rums will have a noticeable burnt flavor resulting
from over-distillation by direct fire.
"Export trade" Jamaica Rum is manufactured principally for
European, especially German, consumption. This class of goods
RUM 145
is so high in flavoring ingredients that it is unsuitable for beverage
use, as such. The chief uses are for blending with lighter rums
or neutral spirits and for the fortification of hock and similar
wines.
Rum Manufacture. Jamaica Rum. Rum is distilled from
the by-products of sucrose recovery from sugar cane juice. The
process of sugar recovery is here stated in brief outline to explain
the origin of the raw materials for rum. The cane, within a
few hours of cutting, is brought to the crushing mill. The lapse
between cutting and crushing must be short to avoid losses of
sucrose from various sources, especially inversion. Hence mills
are usually rather small and serve only a limited territory. The
sucrose content of the sugar cane varies from 10 to \%% of the
total weight.
At the mill the canes are cut into short bits by the rapidly
revolving knives of the cutter and then pass to a series of three-
roll crushers which press out the juice. If no water is added the
process is called "dry crushing.' 1 In u wet crushing 1 ' water is
played on the cane at the second or third set of rollers. The
pressed cane or "bagasse" may be treated for further extraction.
The juice drops into troughs under the rollers and is strained,
warmed to about 200 F. and left for a time in settling tanks.
Some sugar is still retained in the bagasse. Hence in some
plants it is passed on an endless belt through a shallow trough
containing water and then pressed once more in crushing rolls.
This extract is added to the first juice.
The amount of juice in the cane varies according to district of
origin and degree of maturity. About 60 to 80 per cent of the
juice is extracted by the methods described and the juice con-
forms approximately to the following analysis:
per cent
Sucrose 14.1
Reducing sugars 0.6
Water 83.6
Undetermined solids 1.7
100.0
146 BRANDY, RUM, GIN
After settling, the juice, which is still turbid and has an acid
reaction, is drawn into mixing tanks and treated with enough
lime to make it slightly alkaline. This treatment results in the
precipitation of a number of impurities. The limed juice is heated,
and in about an hour albuminous material coagulates on the lime
precipitate forming a crust, and the whole produces a thick scum.
After the juice has settled, the scum is removed and sent to
the fermenting tank in the still house. The clear juice runs to
evaporators, its sucrose content being about 14 per cent. In the
first evaporation, it is concentrated to about 50 per cent sucrose.
Further concentration is carried on until the desired point for
proper crystal growth has been reached. The mass in the pan,
then called "massecuite," contains a total of 82 per cent sucrose
and perhaps 8 per cent water. Of the total sugar in the hot
massecuite 56 per cent is in crystals and 44 per cent is in solu-
tion; after cooling 65 per cent has crystallized and 35 per cent
remains in solution.
The thick semi-solid mass is placed in centrifugal baskets and
"whizzed." The adhering solution which whirls off to the out-
side, is collected and stored as molasses. The crystals are first
washed in the basket, then removed for shipment. They con-
stitute the raw or centrifugal sugar which refineries buy.
The molasses may be concentrated again until all of its crys-
tallizable sugar has been removed.
Fermentation. In the meantime the scum which was sent to
the fermenting pan in the still house was allowed to remain a few
days until it soured, a certain amount of bagasse having been
added to assist souring.
A mash is made up of diluted molasses containing about 25
to 30 per cent sugar and skimmings (sometimes juice is added).
"Dunder" is also added. This is the name given to the spent
liquor from the stills and has the color and consistency of pea-
soup. It contains mineral salts, coagulated albuminoids and
soluble nitrogenous substances; and not only stimulates fermenta-
tion but increases yield and has a distinct influence on taste and
flavor.
The mash as mixed contains about 12 per cent fermentable
RUM 147
sugar. A vigorous fermentation soon sets in as a result of the
sub-tropical climate and the composition of the mash. Fermen-
tation is completed in about 6 to 12 days, sometimes longer,
various organic acids being formed along with the alcohol.
Distillation. Distillation is carried on in pot stills. The
whole process must be carried out with a great deal of care. The
first distillate has a nauseating odor and a raw burning taste so
that it must be rectified to eliminate objectionable ethers, alde-
hydes and acids. It is also customary to trap off a portion of the
total rectified distillate so that it may be used for blending with
succeeding distillates.
Demerara Rum. We are fortunate in having the following
description of rum manufacture which is quoted from a "Com-
munication of the British Guianas Planters Assn. to the British
Royal Commission on Whiskey and The Potable Spirits, 1909."
"In British Guiana the wort is prepared by diluting molasses with
water to a density of 1,060 and it is rendered slightly acid by the addi-
tion of sulfuric acid in quantity sufficient to set free more or less of the
combined organic acids, but so as not to have uncombined sulfuric acid
present in the wash; whilst in some of the distilleries additions of sulfate
of ammonia in small proportions are made to the wash, in order to supply
readily available nitrogenous food for the yeasts and to thus enable them
to multiply with rapidity and to retain a healthy active condition. The
reason for rendering the wash slightly acid is to guard against the exces-
sive propagation of the butyric and lactic organisms, and to render it more
suitable for active alcoholic fermentation. Within a very short time from
the molasses being diluted it enters into vigorous fermentation and rapidly
proceeds to more or less complete attenuation in 30 to 48 hours.
In British Guiana the distilleries are of three kinds:
1. Those using pot stills or vat stills which are practically only
modified stills.
2. Those using both pot stills or vat stills and Coffey or other con-
tinuous rectifying stills.
3. Those using only Coffey or other continuous rectifying stills.
Vat stills consist of cylindrical wooden vessels built of staves strongly
hooped with wrought iron. They have high copper domes covering open-
ings in the heads of the vessels which communicate with a retort or retorts
of the Jamaica pattern, but, as a rule, the retort acts as the lowest vessel
of a rectifying column. As in Winter's still a spiral pipe or a series of
i 4 8 BRANDY, RUM, GIN
small perpendicular pipes descend down the interior of the column through
which cold water is run whenever distillation is in progress, and by which
the spirit vapor undergoes a process of rectification as it ascends the
column before passing into the condenser. Vat stills are heated by injec-
tion of steam."
Aging. The aging of rum does not differ markedly from
the aging of whiskey (q.v.). The temperatures are possibly a
little higher and the time somewhat shorter. Either charred or
uncharred casks are used and a deficiency of color in the finished
product is made up by caramel.
Imitation Rum. The practice of "stretching" rum is quite
common, either of two general methods being used. In the first
method rectified grain alcohol is diluted, "cut," with distilled
water until it is of the same alcoholic strength as a previously
selected rum of strong bouquet. This diluted alcohol is then used
to mix with the rum in any ratio from one-to-one to one-to-four or
five parts of alcohol to one of rum. The mixture is aged in casks
for several months at a temperature of about 75 F. The product
of this treatment might possibly be better called a "cut" rum than
an imitation. In the second method, a mixture prepared as just
described but before aging is further "cut" with distilled water
and redistilled. The new distillate is treated with "rum essence"
and then aged in casks. Rum essence, or the so-called "pelar-
gonic ether" is a mixture of esters, alcohol etc, prepared in various
ways. One favored method is said to consist in distilling a mix-
ture of alcohol, crude acetic acid, starch, manganese dioxide and
sulphuric acid. Rum essence is quite generally used in the prep-
aration of imitation rum and also as a cooking flavor. An ex-
perienced taster, however, would have no difficulty in distinguish-
ing it from the genuine article.
GIN
There are two essential differences between gin and the liquors
which have previously been under consideration. The major dif-
ference is that gin derives the bulk of its flavor from pre-existing
natural essential oils rather than from the products of fermenta-
tion. Secondly, gin is somewhat more of an international product,
GIN 149
being made in the Continent especially Holland, in the British
Isles and in the United States. In each country there are minor
qualities which are distinctive. In general, however, gin is a
colorless beverage containing from 40-55% of alcohol and hav-
ing a perfume-like odor. It was originally made in Holland.
Holland Gin. Since the production of alcohol for gin is a
separate step from the introduction of the flavor it might seem
that any sufficiently pure alcohol could be used in the manufacture
of gin. As far as the American public is concerned, this is prob-
ably true. However, abroad, and especially in Holland, the con-
generic substances of the pot-still distillate from a properly fer-
mented mash of barley malt, rye and corn are required to round
out the taste of the product. This distillate, called moutwjn or
maltwine, is bought from distilleries by the gin manufacturers
and redistilled by the latter through a "gin head" containing
juniper berries and other flavoring materials. This is the ma-
terial which under the various names "Geneva," "Hollands,"
"Hollands Geneva" or "Hollands Gin" has spread widely over
the surface of the earth.
English Gin. In England the same raw materials are used
as in Holland. However, since the distillation of alcohol for use
in gin is almost always done in patent stills, the flavor of the
British gin is decidedly different from the Dutch. The English
gin manufacturer usually requires a clean spirit which has been
rectified until only a slight grain flavoring remains, as decided by
the judgment of the operator. Molasses spirit is objected to both
in England and the Netherlands on the ground that it gives a
coarse flavor to the finished gin. The selected spirit is then made
into gin in a number of ways. The more approved process is
to re-distill the spirit, after dilution with w r ater, in a pot-still
equipped with a gin-head containing juniper berries and other
flavoring materials as required. Some manufacturers, however,
distill the flavoring materials separately and then add them to the
diluted alcohol. Others distill before dilution, etc. The addition
of from 2-4 or even 6% of sugar, or of l /2-i% of glycerin to gin
is common practice to sweeten and "smoothen" the product. Gin
is usually bottled as made and is unaffected by aging.
150 BRANDY, RUM, GIN
American Gin. In the United States gin is made from the
usual grain mash with juniper berries as the principal flavoring
agent. Sloe gin has in addition the flavor and color extracted
from "Black-haw" or Sloe berries. Among the flavoring agents
used in gin are the following:
Angelica Fennel
Anise Grains of Paradise
Bitter Almonds Juniper Berries
Caraway Seed Orris Root
Coriander Liquorice
Calamus Turpentine
Cardamoms Bitter Orange Peel
Cassia Bark
Turpentine is only occasionally used as a substitute for the es-
sential oil of juniper. A small addition of sulphuric acid to the
spirit before rectification is sometimes made to produce an ethe-
real bouquet and flavor.
Gin manufacture in the United States may be carried on along
with the manufacture of whiskey and spirits. Its place in this
unitized operation is shown in Fig. 26. A specialized plant for the
manufacture of gin is shown in Fig. 34. The process is as follows :
Pure spirit from the charge tank is drawn as needed to the gin
still. Sufficient good-quality water is added to dilute the alcohol
to about 125% proof. The juniper berries and other flavors re-
quired for a batch are placed in the gin head. High pressure
steam is run through a coil in the still to cause distillation. The
heads and tails are discarded, and the middle run, after dilution
with distilled water in the blending tank to 80 or 90% proof, is
drawn off to bottles.
Bath-tub Gin. This term was applied during the prohibition
era to so-called u synthetic gin" made by adding mixtures of es-
sential oils or essences to a suitably diluted alcohol. Smootheners
were sometimes added and the product was then ready for the
market. Actually, while the term might have some bearing as
applied to the questionably sanitary methods of small bootleggers,
gin has largely been made in this way in all countries and at most
times. Nor is there any very cogent reason why gin thus made
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iS2 BRANDY, RUM, GIN
"synthetically" should be inferior qua gin to the distilled product.
The question seems to be largely one of taste and we have pre-
viously stated that the taste for gin varies in different countries.
Certainly, the probability is in favor of a synthetic gin being
consistently uniform, batch after batch, and the balance of oils
used as flavors can be so selected that any desired aroma is
achieved.
APPLEJACK
Applejack bears the same relation to cider that grape brandy
bears to wine, but whereas fermented cider is more dealt in abroad
than here; the reverse is true of applejack. It has been stated
that applejack was first made in this country as early as 1698,
and it is still a staple article of commerce.
Applejack is the product resulting from the distillation of fer-
mented apple must. Hence, in general, the same considerations
apply to the manufacture of applejack as to that of grape brandy,
and the same processes are used. It should be noted in par-
ticular that the definition just stated differs from the popular im-
pression of applejack as the unfrozen liquid removed from the
core of a barrel of frozen cider. The product of this latter
process would not only contain the alcohol of the cider, but also
all its other dissolved substances and would be quite unpalatable.
As far as any passable applejack is concerned, only that made
by distillation need be considered, although it is possible that
isolated farmers may in some few cases make their "hard liquor"
in the more primitive fashion.
For the purpose of making applejack it is important that the
cider be made from suitable apples both as regards variety and
quality and that the fermentation be conducted in a manner to
avoid as far as possible the formation of volatile acids especially
acetic acid. The reader is referred to pp. 187-9 on Cider for
further details regarding the fermentation operation. The next
step after the fermentation and aging of the cider is the distilla-
tion of the brandy. Here particularly, the manner of procedure
is similar to that in making grape brandy (q.v. pp. 141-2). Pot
stills are, generally preferred to continuous stills and two or three
ARRACK 153
distillations are used to secure the desired alcoholic strength
coupled with the proper removal of foreshots and tailings, which
contain respectively aldehydes and fusel oil. After distillation
the spirit is aged in oak barrels. Uncharred barrels of well sea-
soned white oak are used, and those which have previously held
wine or other spirits are preferred to new barrels.
It is claimed, that on account of the lower starch and protein
content of an apple must as compared with a whiskey mash,
applejack can be aged in a much shorter time than whiskey. Hence
it is usually considered potable after as little as three to six
months' aging. It is, indeed, further claimed that apple brandy
begins to lose its special character on aging in the wood for more
than four to five years.
ARRACK
Arrack is prepared by distillation from toddy or a mixture
of toddy with either fermented rice or rice and molasses mash.
Toddy is palm wine which is obtained by fermenting the juice of
the cocoanut palm. Arrack ranges from yellow to light brown
in color. Its flavor and aroma resemble those of rum, if much
molasses has been used in its preparation, but not to such an ex-
tent that the one could be substituted for the other without in-
stant discovery. Normally arrack has a sourish aroma and taste
which are claimed to derive from the toddy. The alcoholic con-
tent of arrack ranges from 70 to 80 per cent by volume.
It is used either as such or in the preparation of hot drinks
(grog, punch), particularly in making Swedish Punch, and also
for strengthening and improving the aroma of ginger liqueurs and
bitters such as Angostura, Boonekamp, etc. It is also used in the
preparation of sweetmeats.
Arrack is made in Siam, the Malay Archipelago, East India
and Jamaica.
Manufacturing Process. When rice or rice and molasses are
used it is customary to employ only rice of the highest quality.
Germination of the grain is started by the usual moistening
with water and spreading in heaps or layers. As soon as the
kernels start to sprout the grain is crushed between rollers and
154 BRANDY, RUM, GIN
hot water is added until the temperature of the mash reaches the
neighborhood of 140 F. Around this temperature the enzymes
convert the starch to sugar. The wort is strained and cooled to
approximately 70 F. Fermentation is started by adding either
toddy or a toddy and molasses mixture according to the formula
employed. The fermented wash is subjected to three or more
distillations after fermentation is completed. The unusual num-
ber of distillations is required by the crude and inefficient stills
employed.
VODKA
Genuine vodka is made from a mash of unmalted rye and
either barley or rye malt. Potatoes and corn have been used as
substitutes for rye in the cheaper grades. The alcoholic content
of the better grades ranges from 40 to 60 per cent.
SCHNAPPS AND KORNBRANNTWEIN
These distilled liquors are consumed in considerable quantities
in Germany, Holland and elsewhere on the continent of Europe.
Kornbranntwein is prepared from a mixed mash of malted
and unmalted cereals, generally rye. Corn may also be used.
Methods of manufacture are similar to whiskey processes.
Schnapps is diluted, rectified potato alcohol prepared by ( i )
heating a mash of potatoes under a pressure ranging from 30 to
60 pounds to achieve pastification of the starch; (2) converting
the starch to sugar by mashing with malt; (3) fermenting accord-
ing to standard methods; and (4) distilling so that the final
product is well rectified.
CHAPTER XI
WINE
Definition. The term wine is a very broad one. It includes,
with proper qualifications, the product resulting from the fer-
mentation, with or without the addition of sugar and other sub-
stances, of such diverse materials as dandelion blossoms, elder-
berries, etc. More particularly, however, it refers to the result
of the alcoholic fermentation and other suitable treatments of
grape juice. It is in this sense that we shall use the term here.
The processes by which raw grapes are converted into wine in-
clude crushing, pressing, defecation, fermentation, fining, racking,
fortification, etc. Historically, the preparation of wine is of
immemorial age. As an industry it dates back for more than two
millennia, which of course gives it rank among the oldest of hu-
man occupations.
Classification. Even in the centuries before the Christian
era, qualities of w T ine were distinguished and different grades were
known and demanded by consumers. At the present time and for
commercial use almost innumerable distinctions are made in the
grades and qualities of wine, including naming by types, combined
with geographical distinctions down to the name of a particular
vineyard and further distinction by the year of the vintage. The
brands and names recognized in commerce are to be reckoned by
thousands.
A few citations are given to illustrate this point. Among the
French red wines are many which are highly valued and of whose
excellence there can be but one opinion. These include the red
wines of Burgundy and especially those of Musigny, Richebourg,
Romance, Chambertin, Gorton, Beaune des Hospices, Pommard,
Volnay, Allos du Roy, and Clos Vougeot. The Clos Vougeot
is one of the most highly prized of the products of the beauti-
156 WINE
ful Burgundian vineyards; its origin can be traced back to A.D.
i no when the monks of Cipeaux received the vineyards from
Hugues le Blanc, lord of Vergy, and cultivating with infinite care,
succeeded in producing a wine which has maintained its reputa-
tion for centuries. The wines of Beaujolais such as Macon,
Thomis, Fleuric, and Moulin-a-vent are also known, and the pride
of the banks of the Rhone are I'Hermitage, Cote-Rotie, and Cha-
teauneuf-de-Pape. But the French wines, however, which enjoy
perhaps the greatest popularity in the land which produces them
are the world-famous red wines of Bordeaux. Some of the prin-
cipal varieties of these are Haut Brion, Chateau-Margaux,
Chateau-Leoville, Chateau-Lafite, Chateau-Lagrange, Chateau-
Larose, Chateau-Millet, Mouton-Rothschild, Chateau-Latour,
Branaire, Montrose-Dolfus, Ducru-Beaucailloux, Closd'Issan, St.
Estephe, St. Emilion, and Medoc. Although the wines of Bor-
deaux have been famous for centuries, it was not until towards the
end of the eighteenth century that they became really fashionable,
a state of affairs which was largely brought about by the influence
of Marshal de Richelieu, who introduced them to the notice of the
Parisians.
There are a great many varieties of white wine, and perhaps
the most famous of all is the Rhenish wine known as "Johannis-
berger." This variety has a reputation which is world-wide, and
is said to fetch the highest price among white wines. Enormous
casks of Johannisberger which were casked and stored in their
present position over three centuries ago are lying in the muni-
cipal wine cellars of the township of Bremen. This wine, known as
"the Rose," is as one might suppose, the subject of many legends,
and is offered in hospitality to royalties and other persons of dis-
tinguished rank who partake in the festivities of the town; it is
also graciously given to the sick. Other Rhenish wines of great
repute are Rauenthaler, Liebfraumilch, Marcobrunner, Rudes-
heimer, Hoheheimer, Kottenlocher, Zeitlinger and Riesling.
The white wines of Burgundy are also highly appreciated and
Montrachet is regarded by some as the king of white wines.
Meursault-Goutte-d'Or, Chablis Moutonne, Pouilly-Tuisse are
also excellent. Among the white wines of Bordeaux, Chateau
CLASSIFICATION 157
Yquem is considered the best, and Chateau-Myrat, Latour-
Blanche, Clos St. Marc, and the wines of Sautome, Barsac, and
Graves also enjoy a high reputation.
There are many varieties of champagne, but some of the
most famous are Pommery-Greno, St. Marceaux, G. H. Mumm,
Moet et Chandon, Montebello, Heidsieck, Roederer, Mercier,
Veuve Cliquot, and Lanson.
Most of these names correspond to real differences. Names
taken from regions, such as Rhine wine or Sauterne, represent
large differences in character easily distinguishable by taste and
usually by chemical analysis. Names representing vineyards or
vintage years represent differences of quality, which may be
equally marked to the practiced taster, but are difficult to indicate
by chemical means.
Names drawn from particular vineyards are properly con-
sidered proprietary and should not be used, nor the wines imi-
tated elsewhere. Names drawn from localities or regions are of
the same nature. They represent qualities due to special features
of soil, climate, grape variety, and manufacturing methods which
can not be identically duplicated in any other place. An excep-
tion should probably be made of certain names which, while
originally derived from particular localities have come to repre-
sent, through long usage, characters due principally to methods of
manufacture. Such names are Port, Sherry and Champagne.
The name Burgundy should properly be given only to wine
made in Burgundy from Pinot grapes; the name Medoc only to
wine made in Medoc from Cabernet and also to the three or
four other varieties recognized there as capable of producing the
wine to which the region owes its reputation.
There seems to be no sufficient reason, however, why a wine
should not be called Port if it is made of suitable grapes in the
recognized way and resembles those wines of the banks of the
Douro, which first received this name. "Port," is no longer synon-
ymous with "wine of Oporto." All the wines made in the region
of Oporto are not port, nor does all port come from that region.
With these possible exceptions, locality names belong only to
the wines produced in that locality. Not only is this fair to the
158 WINE
consumer, but it is sound policy in the selfish interest of the pro-
ducer. Wines are produced most profitably by those localities
which have an established reputation. They have a sure market
whatever the abundance of crops in other localities. It should
be the aim of each locality to obtain and maintain a reputation
which will make it independent of general competition. This can
be done only by marketing consistently good wines under the
name of the locality.
The listing of wines in the manner indicated, while exceed-
ingly important to the consumer of wines and especially to the
connoisseur, is of little aid to the student or technician. For-
tunately, it is possible to classify wines also in a more general
manner on a basis of their gross composition, disregarding the
fine distinctions made by the specialist. There are four dicho-
tpmous bases on which wines can be divided, namely:
1 . Dry or sweet
2. Fortified or unfortified
3. Sparkling or still
4. Red or white
These classes are defined as follows:
a. Dry wines are those in which practically all of the sugar
has been converted by fermentation into alcohol. Usually they
are of comparatively low alcoholic content (ca. 8-12%). This
class includes such wines as Chablis, Riesling, Hock, Moselle,
Claret, Burgundy, Gregnolino, and Chianti.
b. Sweet wines contain some unfcrmcnted sugar and have
an alcoholic content usually between 13-15% by weight, all of
which has been produced by fermentation. Auslese Rhine wine,
Sauterne, and Tokay are wines of this class.
c. Unfortified wines are those whose alcoholic content is en-
tirely derived from fermentation. All of the wines mentioned in
classes a. and b. fall within this group.
d. Fortified wines derive some of their alcoholic content from
fermentation and some from the addition of distilled spirits, usu-
ally grape brandy. They contain usually from 1 8-22% of alcohol.
Madeira, malaga, muscatel, port and sherry are wines of this
CLASSIFICATION 159
class. Champagnes also fall into this group. Angelicas are some-
times considered to belong to this group although strictly speak-
ing they are not wines at all, since they are made by adding suf-
ficient grape brandy to fresh grape juice entirely to prevent any
fermentation.
e. Still wines, which include most of those mentioned above,
are those whose fermentation has been completed before bot-
tling so that they contain only such proportion of the carbon-
dioxide produced in the fermentation as can remain dissolved in
the liquid in equilibrium with the air under the conditions of
manipulation.
f. Sparkling wines are bottled before the fermentation has
ceased so that they contain carbon-dioxide gas in solution at
greater than atmospheric pressure. When they are served, the
carbon-dioxide is liberated with effervescence. Their gas and
alcoholic content vary according to the market for which they are
intended. They may be dry or sweet, light or strong. Cham-
pagne, sparkling Burgundy, and Asti-Spumanti are examples of
sparkling wines.
g. Red wines are those in which the skins, stems, etc., of the
grapes are present during the fermentation so that the grape pig-
ment is extracted and colors the fermented juice. This group in-
cludes the majority of wines as, for example, Claret, Burgundy,
Port, Chianti, etc.
It should be particularly noted that the distinction between
red wines and white is based on a difference in manufacturing
process. This is of significance on the one hand because the varia-
tion in color of so-called red wines covers every possible tint from
inky purple to pale pink and tan, and on the other hand because
the inclusion of skins, stems etc., in the fermenting liquor leads
to somewhat different composition of the wine and requires dif-
ferent handling from white wines.
h. White wines are produced by fermentation of the grape
juice only, with removal of the marc (skins, stems, etc.) before
the fermentation has proceeded to a point when the pigment be-
comes soluble. Riesling, sauterne, and champagne may be cited
as examples.
160 WINE
It will be seen that by combination of the classes just given,
sixteen possible categories are obtained into which wines may be
classified. For instance, claret is a dry, unfortified, still, red wine.
However, champagne may be a fortified, sparkling, white,
either sweet or dry wine and many other wines can be placed
in more than one category. Despite this ambiguity, these cate-
gories are sufficient for scientific purposes, being based partly on
the nature of the raw material, partly on the composition of the
wine and partly on the methods of manufacture.
A further subdivision of wines may be made within any of the
groups mentioned, on the basis of quality, into three grades: fine,
ordinary, and blending wines. A fine wine is one, all the com-
ponents of which are in proper and harmonious proportion, and
which has sufficient quality to repay aging and bottling. These
constitute, in most regions, only a small part of the product. They
are, however, the ideal toward which the efforts of every wine-
maker tend. Ordinary wines are those which are sufficiently har-
monious in their composition for direct consumption, but which
exhibit no great delicacy of flavor or bouquet. These are usu-
ally destined for bulk shipments and cheap markets. Blending
wines are of various degrees of quality and character, but agree
in having a deficiency or excess of some one or more essential
components. There are blending wines with an excess of alcohol,
or extract, or color which make them unsuitable for direct con-
sumption. They serve, by blending, to correct other wines which
are deficient in these components. Where the wine handlers have
perfected their business, the bulk of wines are used for blending,
for it is only the exceptional wines which cannot be improved by
additions to correct their deficiencies and faults.
Functions of Wine. The experience of many centuries has
taught mankind that wines, when used in proper combination with
foods, not only enhance the flavors of the food and the enjoyment
in partaking of them, but aid in the digestion. There follows
an abridged tabulation of the principal classes of wine together
with the foods they should accompany:
Dry white wines
Oysters, fish, fowl, turkey, vegetarian dinners, omelettes, etc.
MANUFACTURE OF WINE 161
Dry red wines
Roast meats such as beef, pork, lamb, steaks and chops, duck, goose,
turkey, pheasant, venison, etc.; Italian dishes such as spaghetti,
ravioli, macaroni, etc.
Sparkling wines
These are the proper accompaniment of the end of the meal, sweets
and cheese.
Fortified wines
Sherry is preferred to any cocktail by almost all peoples but the
American. It is also the proper wine to serve with soups and with
hors d'oeuvre. Port and other heavy wines like Malaga, etc., are
sipping rather than drinking wines, and should be used with cir-
cumspection during the evening, when the appetite no longer
clamors and the excellencies of the wine can be savored slowly.
In fine cooking, wines play an important part which largely
forms the basis of the reputation of the French cuisine.
MANUFACTURE OF WINE
Introductory. The manufacture of wine is, in principle, a
matter of the greatest simplicity. The grapes are crushed, the
juice fermented, the sludge of exhausted yeast and precipitated
matter is removed by decantation, and one has wine. Unfor-
tunately, there is an equal probability that if no more than the
above is done, the product will be vinegar or something equally
unpotable. Much more must be done if the wine is to be of a
high quality. The ultimate in quality, of course, the wines that
elderly connoisseurs sip with tears of thankfulness, are dependent
not only on full and thorough care in their processing but also on
a combination of favorable weather, soil, etc. in a given year in
a given locality. These accidental factors are beyond human con-
trol. The control of the stated steps in production of wine is,
however, readily feasible and will be the subject of the immedi-
ately following pages.
Components. The fine points of wine making are necessi-
tated by the original composition of the fermenting mass and
the nature of changes which may occur during the fermentation
and after-processes. The must (fresh pressed juice) contains
162
WINE
sugar, organic acids, tannin, flavoring substances, proteins, mineral
salts, and pectin and mucilaginous substances which it derives from
the grapes. It also contains a large variety of yeasts, bacteria,
and fungi, some of which are favorable and some the reverse. An
average composition is indicated in the following Table IX re-
ported by Koenig:
TABLE IX. ANALYSIS OF WINE MUSTS
Other
Nitro-
non-
Sp. gr.
Water
genous
Sugar
Acid
nitro-
Ash
matter
genous
%
%
%
%
matter
%
Minimum. . .
i . 0690
5^-53
O.II
12.89
O.2O
1.68
O.2O
Maximum. . .
1.2075
82.10
0.57
35-45
1.18
11.62
0.63
Average
I . 1024
74 40
o 28
IQ 71
o 64
4.48
0.40
These components and their changes are very largely interrelated.
When the sugar content is high enough the activity of the
first fermentation prevents much action by harmful organisms.
Later, enough alcohol has been produced to prevent the growth
of these. A proper sugar content lies between 18 and 28%.
Organic acids, especially tartaric, serve to produce sound and
healthy wine in a number of ways. Sufficient acidity encourages
sound fermentation and inhibits the growth of the disease bac-
teria. Sufficient acid ensures a full tasting wine which will store
well, while insufficient acid means a flat taste and short life. Acid
also ensures a better extraction of color from the skins.
Tannin, which is derived by extraction from the skins, seeds
and stems of the grape is an essential constituent of the wine. It
serves to confer disease resistance on the wine, aids remarkably
in the clarification and produces a more brilliant color. On the
other hand, an excess of tannin confers an astringence on the
wine which delays its final maturity, although in the end the wine
is more mellow for it.
The flavoring substances present in the raw grapes undergo
MANUFACTURE OF WINE
163
many changes during the life of the wine. To some extent they
control the flavor of the end product. However, the extent of the
changes has never been followed completely by chemical research
so that little can be said on this topic. The characteristic bouquet
of the finished wine is only slightly due to methyl-anthranilate,
which has the distinguishing character of fresh grapes. Various
aliphatic ethyl esters are formed as the wine lives, and these, the
FIG. 35. Corner of the still room in a large applejack distillery. Showing one
of the pot stills. (Courtesy of the American Wine and Liquor Journal,
New York.)
action of special varieties of Avine yeast (S. Ellipsoideus] , and
even of frost (as in Reislings) each contribute their share to the
final celestial bouquet of good wine.
The relation of the constituents of the raw must to the fin-
ished wine is shown in Figures 35, 35a.
Red Wines. The production of wine falls naturally into two
broad divisions, red and white wines respectively. The produc-
tion of champagne and of other fortified wines may follow in
164
WINE
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^^ r*^ 4 S
Juliffli
> "i'JSIf
s I ?1
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MANUFACTURE OF WINE 165
their earlier stages either of the broad divisions stated and
diverges only at the later stages. The apparent divergence be-
tween red and white wine processes consists only in that for the
former, fermentation precedes drawing off and pressing, while
for white wines the order is reversed. Actually, other differences
are entailed which will be discussed under the topic of white wine
manufacture. Red wine manufacture is somewhat simpler and
will be considered here.
The sequence of operations in the manufacture of red wines
is indicated in the flow sheet, Fig. 36.
Grape Bunches
Stemming (Partial or complete)
Crushing
i t I (optional)
Fermentation > j Sterilization by Sulphur Dioxide and
I [ Starting with Cultured Yeast
Drawing Down and Pressing
First Ripening and Secondary Fermentation
J, (optional)
Second Ripening > Fining, filtration, etc.
J, (optional)
Bottling or Cask Ripening > Pasturization
FIG. 36. Flow Sheet of red wine manufacture.
When the grapes are at the proper stage of ripeness the
bunches are plucked and brought to the winery. This may vary
in size from the home of the French peasant to the large com-
mercial wineries with capacities for thousands of gallons of wine.
There can be, at this stage, no delay, since the grapes may become
infected if left piled in bunches. The next stages to the starting
of the fermentation must follow in rapid order.
Stemming. If stemming is practiced, it may be done by
hand, by the use of a screen which will pass the grapes, but not
the stems, and which may be operated manually with the aid of a
rake to spread the grapes over it, or may be mechanically shaken
or vibrated. Another means of stemming, is a machine compris-
ing a stationary, horizontal, perforated metal cylinder fitted in-
ternally with a revolving shaft having arms which cause the
1 66 WINE
grapes to travel along the cylinder and drop through the holes
or slots in its wall. Stemming may also be done after crushing.
A strainer of suitable size with proper openings and fitted with
revolving blades serves this purpose excellently.
The stems can furmsh tannin to the juice if the skin and
seeds are deficient in this respect. However, they also contain
substances which "brown" the color and spoil the flavor of the
finished wine. They may also introduce difficulties in handling
the crushed mass.
Crushing. In order to liberate the juice of the grapes and
inoculate it with yeast, it is necessary that the grapes be crushed.
Probably a sort of pestle or stamper operated in a container
is even now used to crush grapes in small lots. By far the great-
est amount, however, are crushed in a roll machine. This con-
sists of a hopper into which the grapes are placed and from which
they feed between two grooved rolls turning toward each other
at different rates of rotation. The grooves catch the grapes from
the hopper, and one roll passes over grapes held in the grooves
of the other, crushing them. The crushed grapes may fall
directly into the fermenting vat, or into a tank whence they may
be pumped to the proper vat. In adjusting the machine it is only
necessary that the rolls be so spaced that the seeds pass through
uncrushed. Roll crushers are available in any size desired, from
the domestic "one lug n to the large machines found in California.
In any case their capacity is usually great compared with vat
and other facilities required in the winery. There are possibly
still existing, and there certainly were in the past, rural districts
in which the grapes were placed directly in the fermenting vat,
and the crushing done by the bare feet of men and women who
walked around on the mass.
Fermentation. The general considerations involved in the
fermentation of grapes to produce wine have been discussed in
Chapters V and VI. The fermentation of the crushed grapes
is started as desired, either naturally or by means of a starter,
and means to control the temperature must be available if very
large batches are being fermented. These may include water
cooling coils or as in parts of California, the construction of
MANUFACTURE OF WINE 167
the vats with thin cement concrete walls so the evaporation serves
to effect some cooling. Even chloroforming the yeasts, tem-
porarily to arrest the fermentation and stop heat production has
been attempted. This control of temperature, it is repeated for
emphasis, is necessary because the desired yeasts function best
FIG. 37. Redwood tanks. 17,000-25,000 gallons capacity. (Courtesy of the Amer-
ican Wine and Liquor Journal, New York.)
between 70 and 80 F. while the disease bacteria are favored
by temperatures over 90. It should be noted, however, that
yeasts can be "trained" to work at unusually low or high tem-
peratures when the climate, as in Southern California, requires
it. The first visible evidence of active fermentation is the forma-
tion of carbon dioxide. This is liberated in bubbles which become
entrapped in the skins and cause them to rise and mat at the top
1 68 WINE
of the vat forming a "cap." When this cap is exposed to the
air, the upper surface of the cap quickly ferments to completion
and offers an excellent start to vinegar bacilli. At the same
time the grape pigment becomes oxidized and bleached. To
avoid this there are two alternative practices. The cap may be
broken up and pushed down manually, or even as in some dis-
tricts in France trodden down by men who enter the vats stripped,
for this purpose. Alternatively a grid is installed in the vat about
six inches below the level of the must, to keep the cap submerged.
In this case it is necessary, to obtain aeration and uniform fer-
mentation, that the liquor be circulated by pumping it from the
bottom of the vat and allowing it to pour back at the top. A com-
bination of these systems is often favored. The fermentation is
kept open until the yeasts have multiplied and developed strongly
and then the cap is submerged to avoid the dangers of open
fermentation.
Changes During Fermentation. While the most marked
change during fermentation is the conversion of grape sugar into
alcohol and carbon dioxide, other changes of smaller magnitude
but equal importance to the quality of the finished wine also
occur.
As indicated previously, some of the acid present in the fresh
must is consumed by the yeast. The drop in acidity is about
40%, or from an original acidity of 0.5-1.5% expressed as tar-
taric, to an acidity of 0.3-0.7% in the finished wine. This in-
cludes volatile acids formed which should not exceed 0.15%.
Protein matter present in the grapes is also partly consumed
during fermentation. The manner of this consumption was dis-
cussed in Chapter V. The end products, organic acids, esterify
with the alcohol of the wine and contribute largely to its bouquet.
The liquid extracts tannin and coloring matter from the skins
and seeds of the grapes. The former, as previously stated, is of
great importance to the soundness and clarity of the wine. The
coloring matter of the grapes is, of course, the obvious distin-
guishing feature of red wine. This color includes a group of sub-
stances of obscure composition, which are called enolic acids.
They probably do not go into complete solution in the liquid, but
MANUFACTURE OF WINE 169
rather into colloidal solution. Hence, the cell walls of the grapes
must be broken down either by fermentation or heating (as in
making bottled grape juice) before the color dissolves. It is
possible that the alcohol may also have something to do with dis-
solving the color. Over-ripe grapes, in which it is possible that
the pigment is over-oxidized, yield a paler wine than those in
which the grapes were gathered at the peak of their ripeness.
Many other known and unknown changes of minor importance
occur during the fermentation even when it is running its proper
course. Coagulation of a portion of the albuminous and pecti-
nous substance present may be mentioned as an example. How-
ever, the main changes have been indicated and the key to all is
the conversion of sugar to alcohol.
Completion of First Fermentation. The rate of this con-
version varies, as might readily be foretold, with the temperature,
the vigor and numbers, and the strain of yeast. At the best,
about 4 per cent of sugar per day is converted, so that a must
containing originally 20% of sugar, will be fermented dry in about
five days. Actually the time required may be anything between
three days and three weeks.
At some time during the active fermentation or very shortly
after its completion the fermented juice or new wine must be
separated from the marc, the pressed residue of grape skins and
pulp. The exact stage at which this is done is very largely a mat-
ter of pure choice although to some slight extent climatic factors
serve as a guide. In the French Bordeaux district pressing is not
done until two or three weeks after the end of the violent fer-
mentation on the theory that thereby strength is added to the
wine. In the Burgundy district a reverse theory is held that the
shorter the fermentation the better the wine. Hence no time is
lost between the completion of the fermentation and the separa-
tion of new wine from marc. Here in the United States it is the
general custom to draw down and press even before the com-
pletion of fermentation. It is stated that in the Sandusky win-
eries there was often as much as ten per cent of sugar in the must
at the time of pressing. All three practices will produce good
wines. Like the choice between open, submerged or combined
170 WINE
fermentation, the election probably depends on the judgment and
skill of the wine maker.
Pressing. Once the choice of time has been made, the mode
of separation between new wine and marc remains essentially
the same. By openirig a tap at the bottom of the fermenting vat,
a very considerable portion of the new wine will drain off with-
out pressing. This portion of the yield is usually less harsh and
matures more rapidly than the press juice. Hence it is usually
kept separate from succeeding portions of juice.
When the drainage is essentially complete, the remaining
saturated mass is transferred to a press. These range from small
hand-screw affairs to large hydraulic presses. Their principle of
operation is nevertheless identical with that of the old home
jelly-bag. The mass is placed in a press and the solid matter
confined within a strong porous cloth, the filter cloth. When
pressure is applied the new wine is squeezed out and the solids
remain in the cloth. In order to avoid clogging of the pores of
the cloth by the finer portions of albuminous and other matter in
the mass, it is essential that pressure be applied gradually al-
though it may finally be exerted to the limit of the machine used.
Even with this precaution, it is usual to open the press, loosen
the mass and repeat the pressing once or twice. Some of the
wineries which are more interested in quantity than quality of
product, moisten the residue in the press with water, before the
third pressing to wash out as much extractable matter as possible.
This last pressing is called pinette in France and may not be sold.
Aging and Racking. The new wine produced in the manner
described is still far from the finished product which is mar-
keted. It is low in alcohol and it still contains unfermented sugar,
excess tartaric acid and tannin in solution. It is cloudy due to the
presence of suspended yeast cells, albuminoids, pectinous mate-
rials, etc. Its flavor is harsh and the aroma quite grapey rather
than winey. Time is required for the completion of fermentation,
the settling of suspended solids, and the ripening of the flavor.
Usually these processes are accomplished by storing the new
wine in oak casks at a cool temperature (50 F.) during the win-
ter. A great deal of settling takes place, aided by the formation
MANUFACTURE OF WINE 171
of cream of tartar (potassium acid tartrate) crystals. With the
spring and approach of warm weather, the wine is "racked." That
FIG. 38. Modern wine storage room. (Courtesy of the American Wine and Liquor
Journal, New York.)
is, it is carefully poured or siphoned off from the sediment into
new clean casks. The importance of this process is much greater
172 WINE
than appears from its simplicity. During the racking, some aera-
tion takes place resulting in the solution of oxygen in the wine.
This oxygen acts on the remaining albuminoids in the wine to
precipitate them. It also improves the color and flavor. If the
wine is to be fortified, the alcohol is added in portions at each
racking. Artificial aeration is often employed to accelerate the
processes desired. The sequence of aging and racking is re-
peated at intervals of a month to six months until the wine is
ready for bottling.
Modifications in the temperature of storage, etc., all have
their effect on the wine. Madeiras and sherries, for example, owe
their special flavors to aging at a higher temperature than is
usual for other wines. Some special wines may have sugar or
condensed must added to them at the racking. For the simple red
wines two or three rackings at intervals of six months are gen-
erally sufficient to produce a satisfactory wine.
Once the wine has ripened satisfactorily, efforts are made to
arrest any further changes. Usually this requires that the wines
be bottled and thereafter stored in a cool place with a minimum
of disturbance. Sometimes the wine is pasteurized before bot-
tling. This consists in heating it briefly to kill off as many bac-
teria as possible. The difficulty is always that more heat or time
of exposure are required for complete sterilization than the flavor
of the wine will permit without harm. Hence a compromise is
made. Pasteurization temperatures range from I2o-i5o F.
and times from a very few seconds at the higher temperatures
to a quarter hour at the lower heats. The entire operation is
one which can only be performed on a large scale with the best
possible equipment and control. Fortunately the dairy industry
has furnished various machine designs and the technique of their
operation which can be transferred unchanged to the wine
industry.
WHITE WINES
In general the manufacture of white wines is very similar to
that of red. The basic difference as will be noted by comparison
of the flow sheet for red wines, Fig. 36, and a similar flow sheet
WHITE WINES 173
for white wines, Fig. 39, is that red wines are fermented on the
whole crushed mass, while white wines are pressed before fer-
mentation so that only the juice is fermented.
This basic difference necessitates other variations between the
manufacture of red wine and that of white. The plucking and
pressing operations are the same. Since there has been no fer-
mentation to break down the walls of the grape cells, higher pres-
sures are required to ensure a good extraction of juice.
Sterilization. Most of the wine yeasts are found on the skins
of the grapes and remain there during the pressing. Hence the
fresh grape juice is deficient in yeast and would ferment slowly
Grape Bunches
Stemming (Partial or Complete)
T
Crushing
Pressing
4'
Sterilization with Sulphur Dioxide
Fermentation started with Cultured Yeast
First Ripening and Secondary Fermentation
I (optional)
Second Ripening > Fining, filtration, etc.
| (optional)
Bottling or Cask Ripening * Pasteurization
FIG. 39. Flow sheet of white wine manufacture.
and poorly if only the natural yeast were relied on to cause
fermentation. During this long slow process, disease bacteria
would have ample opportunity to flourish and spoil the wine, es-
pecially since little or no alcohol is present, the acid is low and
the tannin which comes from the skins and seeds is also very
low. Hence it is preferable and indeed almost essential that the
must or press juice be sterilized and then re-started with fresh
vigorous yeast culture. The usual manner of sterilization is by
means of sulphur dioxide which is introduced generally by burn-
ing sulphur in the cask into which the must will be placed.
The usual way of burning sulphur in a cask is to use sulphur
matches or tapes, which are strips of thin cotton cloth which have
174 WINE
been dipped several times in melted sulphur. These tapes are
hung on an iron wire about eighteen inches long, bent up at one
end to hold the tape and fastened to a bung at the other. This
method has the defect that some of the sulphur melts and drips
on to the bottom of the vat, where it is incompletely burned. This
incompletely burned sulphur may communicate a bad taste to the
wine. The same is true of the burning of the cloth to which the
sulphur is attached. A better method is to use thin paper instead
of cloth for the tapes and to burn them in a sulphur cage. A
sulphur cage is simply a hollow cylinder of iron, or better, of
porcelain, open on top and closed below, sufficiently narrow to
enter the bunghole and sufficiently long to hold the required
amount of sulphur tape. The cylinder is pierced with numerous
holes in all parts except the bottom inch, which acts as a cup to
catch all the melted sulphur. The cylinder is suspended at eigh-
teen inches below the head of the vat by means of a piece of iron
wire attached to a bung. An alternative method is to add to
the must a suitable amount (about one one-hundredth of i%,
0.01%) of potassium metabisulphite (K2S2O5). This com-
pound contains 56% of sulphur dioxide in an available form and
therefore furnishes a more controllable means of dosing the wine
than does burning sulphur. The effect of this addition is to kill
off harmful bacteria and temporarily to inactivate the yeast.
Hence the must is inactive for a time and may be clarified by
filtration, centrifuging in a cream separator, or even by settling
and decantation. The latter process, which is generally used only
in the smaller wineries, must be performed within 24 hours of the
addition of sulphur dioxide so that the commencement of fer-
mentation by the yeasts still present in the residue does not stir
up the sediment again.
The sterilized and clarified must is now ready for its fermen-
tation. An active culture of yeast is added in about a proportion
of 2-10% by volume of the must. The temperature must be
raised if necessary to 80 F. so that the yeast multiplies rapidly
and continues its activity until enough alcohol is formed to protect
the wine against disease. In small wineries heating is done by
suspending a milk can or bucket of hot water in the must. The
WHITE WINES 175
large wineries are equipped with special coils in the vats which
may be used. In any case, the manufacture of white wine, on
account of its lower acid and tannin content, and on account of
its slower fermentation requires greater care than does the manu-
facture of red wine.
Aging and Racking. In these processes again, greater pre-
cautions are necessary for white wine than for red, and the rack-
ing must be performed a greater number of times and at shorter
intervals to ensure health in the delicate constitution of the white
wines. Similarly pasteurization is almost obligatory for the
lighter white wines prior to bottling.
Correction of Wines. From the time the grapes are crushed
until the wine is bottled any number of inherent deficiencies may
appear or new troubles and diseases may develop. It is the object
of the correction of wines to so alter the deficient or diseased
character that a normal wine results. Very many treatments
have naturally been developed as part of the wine-makers' tech-
nique, for this purpose. Most of them are of limited or occasional
application, but there are four or five which are very generally
required. These include the correction of deficient sugar, acidity,
and tannin, and the fining of wine.
When the grapes are crushed a portion of juice is tested for
its sugar and acid content. A proper sugar content should be
between 20 and 28% and a deficiency requires only a simple cal-
culation and the addition of the calculated amount of ordinary
cane sugar.
The normal acidity of the juice should be 0.5-1.5% expressed
as tartaric. It was formerly the practice to correct low acidity by
the addition of calcium sulphate, Plaster of Paris. Hence the
operation is called "plastering the wine." This treatment has
the advantage of ease since an excess of plaster may be added
and comparatively small amounts as required will react. The
reaction takes place as follows :
Potassium
Calcium Sulphate Cream of Tartar Calcium Tartrate Acid Sulphate
(Insoluble) (Insoluble) (Insoluble) (Soluble)
CaS0 4 + KH(C 4 H 4 O 6 ) - Ca(C 4 H 4 O 6 ) + KHSO 4
176 WINE
The effect, therefore, is to increase the amount of acid in solu-
tion. On the other hand, the practice is undesirable since the
dosage cannot be measured readily and also because it may result
in the presence of sulphates in excess of the legal limits in the
wine (corresponding to 2 grams of potassium sulphate per liter
0.2%). It is easier to correct deficient acidity by blending with
a juice of excess acidity or by the addition of a properly deter-
mined and calculated dose of tartaric acid.
Excess acidity within reasonable limits is not important since
on aging the excess will precipitate as cream of tartar. How-
ever, a new wine with excess acidity is harsh and matures slowly.
There are two procedures which may be employed to correct excess
acidity. These are called respectively "galHzingf* and "chaptaliz-
ing." Gallizing consists in diluting the must with water and add-
ing either grape or cane sugar to correct the deficiency in sugar
which results. Within narrow limits it is a harmless practice,
but naturally, the other essentials of the wine are equally diluted
and a more watery wine results. Chaptalizing consists in partly
neutralizing the acid with chalk and adding sugar. This is usu-
ally done with grapes that are insufficiently mature. Like galliz-
ing it is not objectionable if practiced in great moderation.
Few red wines need treatment for insufficient tannin since
they ferment over the seeds and skins and possibly some stems so
that they have ample opportunity to acquire the tannin they need.
White wines, on the other hand, are almost invariably deficient
in tannin as the pressing immediately after the crushing offers
no opportunity for extraction. The amount of tannin required
in the finished wine is very slight, most of the excess being con-
sumed in precipitating the albuminoids of the freshly fermented
wine. However, the presence of tannin helps ensure a sound
fermentation and to clarify the wine afterward, so that a slight
addition of tannin, say one part to 20,000 of white wine must is
unobjectionable and almost invariably beneficial.
Fining. One of the qualities especially desired of wine is
clarity in the highest degree. The various suspended solids which
interfere with this clarity may settle out during aging and be
removed in racking. Indeed, it has been stated that frequent
WHITE WINES 177
racking of wine is practically the equivalent of both filtration and
sterilization. However, it often happens that the solids are so
finely divided that they do not flocculate or clump together in
sufficient mass to settle out. When this happens the wine remains
cloudy unless an agent is added which will assist the flocculation
and settling. This operation is called "fining." There are a
number of materials which are adapted for this purpose all of
them being gelatinous in nature. That is, they first dissolve in the
wine, then gradually they combine with the tannin, to form in-
soluble tannates which entrap the other solids dispersed in the
liquid and cause the whole to settle to the bottom. Milk is used
for this purpose, especially for wines deficient in tannin as the
milk casein requires only acidity to cause it to change from a dis-
solved to an insoluble state. More commonly gelatin, egg white,
and isinglass are used. Mechanical filtration, refrigeration, and
centrifuging are all coming into use to effect clarification of the
wine.
Bogue, The Chemistry and Technology of Gelatin and Glue,
(1922, p. 355) discusses as follows the use of isinglass for fining:
"The efficacy of the isinglass for this service lies in the purely mechan-
ical property it possesses of maintaining a fibrous structure in the solu-
tion, and as this settles slowly to the bottom it entangles in its netlike
meshes the colloidal bodies that produce the undesirable turbidity. For
clarifying wine the isinglass is first swollen in water and then in the wine
until it is completely swollen and transparent. It is then thoroughly
beaten into a small amount of the wine, strained through a linen cloth,
and stirred into the rest of the wine. The temperature is kept low and
the isinglass does not go into solution, but only into a very finely divided
suspension. Thus the original fibrous structure of the sounds has at no
time since it came from the fish been lost. In this lies the difference in
the action of isinglass and gelatin for fining. If isinglass were heated and
made into a true gelatin it would then have lost the properties which
make it so valuable for this service."
A single ounce of isinglass will clarify, under the optimum
conditions, 500 gallons of wine in 10 days. One ounce of gelatin
will clarify 50-120 gallons of red wine. The white of an egg
will fine about 10 gallons of red wine. This last material is
chiefly used with only the highest quality of wine.
178 WINE
Finings may be prepared as follows :
Gelatin
Cover with wine and soak a few hours or overnight. Dissolve
by gentle heating, cool and dilute with more wine. Mix thor-
oughly and add with stirring to the wine in the cask.
Egg White
Beat to a foam. Allow to settle and filter through heavy
linen. Stir up with a small amount of wine and add with stir-
ring to the wine in the cask.
CHAMPAGNE
General Statement. Champagne is a sparkling wine of fine
flavor and fragrant bouquet. Its effect upon the human system
is the production of rapid, but transient, intoxication. Medical
authorities have stated that fine, dry champagnes are among the
safest wines that can be consumed. Champagne is said to have
valuable medicinal properties and to be of definite benefit in the
treatment of neuralgia, influenza and a run-down condition.
About the time of the Civil War pink or rose-colored cham-
pagnes were fashionable; the color being obtained by tinting with
a small amount of a dark red wine. Today, a straw color is
favored and that is the color of all current commercial cham-
pagnes. Occasionally, a pinkish wine is met, which owes its color
to partial extraction from the grape skins and is the result of
accident rather than design.
Champagnes are made dry or sweet, light or strong accord-
ing to the markets for which they are designed. A dry cham-
pagne, of good quality and fragrant bouquet, free from added
spirit, is made from the best vinbrut, to which a very small
amount of liqueur has been added. Sweet champagne receives a
heavier dosage of liqueur, which hides its original character and
flavor, and therefore can be made from wine of less delicate
flavor.
CHAMPAGNE 179
The dosage of champagne with syrup (liqueur) materially
contributes to its sparkle, effervescence and explosiveness. It is
not true, however, that the heavier the dosage the better the
wine. Too heavy dosage causes an accumulation of carbon diox-
ide in the space between the wine and the cork and such a cham-
pagne explodes loudly and effervesces turbulently when the cork
is withdrawn, but soon becomes flat and loses the characteristics
one looks for in a good wine. On the other hand, a fine dry
wine does not explode so violently, nor effervesce so turbulently,
because it acquires its sparkle to a large extent from the natural
sugar of the grape. This holds the carbon dioxide somewhat
more firmly within the wine and so it continues to sparkle for a
much longer time. While this helps it to hold the characteristics
of a good wine for a longer period, it is only fair to say that a
good champagne should retain its fine flavor even after the carbon
dioxide is exhausted.
Russia and Germany prefer sweet champagnes and twenty or
more per cent of liqueur in the wine is not unusual for the latter
country. England buys very dry, sparkling wines, having about
one-fourth the amount of dosage given wines intended for Ger-
many. France, herself, prefers light and moderately sweet wines.
The United States used to buy a wine of intermediate character
before prohibition. Australia and South Africa like their cham-
pagne strong, while India and China and all hot countries favor
light dry wines.
Champagne is made in Germany and the United States, but
France is commonly considered the home of this king among
wines. The heart of the industry is in the Department of the
Marne and centers around the cities of Reims, Epernay, Ay,
Mareuil, Pierry, Avise, and to a lesser extent, Chalons.
The best American sparkling wines come from the Finger
Lake district of New York, and the Ohio region around Cin-
cinnati. Very little sparkling wine was made in California before
prohibition, but the industry is now being developed there.
Apart from incessant labor, skill, care and precaution the fine
quality of French champagnes is attributed to the climate (which
imparts a delicate sweetness and aroma, combined with finesse and
i8o
WINE
lightness to the wine) and to careful selection of the vines, of
which four types are cultivated, three of them yielding black and
one white grapes. The soil is also said to impart a special quality
which it has been found impossible to imitate in any other part
of the earth. Claims are made that to the wine of Ay it imparts
a peach flavor, to that of Avenay a strawberry flavor, to that of
Graces
Pressing
Pulp -<-
^Juice from second
and third pressing
to inferior wines
Primary
Fermentation
Secondary
Fermentation
Racking and Fining
Blending
(Cuyee)
Finings -
__Pure crystallized sugar
added if cuvee is low in
sugar
- Pure culture yeast
Syrup liqueur and
brandy
-Tannin
Settling
Bottling
Resting
Uncorking, dosing
and corking
Resting
Shipping
FlG. 40.
Hautvillers a nutty flavor, and to that of Pierry a flint taste
known as the "pierre a fusil" flavor.
Manufacturing Process. Figure 40 is a graphical presenta-
tion of the process of champagne manufacture. It will be noted
that the early stages of the process are similar to those of white
wine manufacture excepting that the juice of the first pressing is
kept apart for first quality wines. Second and third pressings
CHAMPAGNE 181
are given, but the wine made from second or third juices is
inferior.
Following pressing the must is drawn into large vats and al-
lowed to rest for 24 hours so that some settling of the sediment
can take place.
It is then transferred to sterilized casks of about 40 gallons
capacity. The cask is filled to about nine-tenths of its capacity,
and the bunghole is generally covered with a vine leaf held in
place by a small stone.
The must is then taken to one of the large underground
caverns or cellars where a temperature of 60 to 70 F. usually
prevails. The cask is bunged up, primary fermentation sets in
and is almost completed in about two weeks to a month depending
on whether the wine is high or low in sugar. At the proper
point, as explained under red wine manufacture, primary fer-
mentation is arrested by filling the cask up to the top, bunging it,
and transferring it to a cooler cellar. Here a secondary and
slower fermentation sets in. The object of this treatment is to
preserve some of the sugar unsplit in order to insure to the wine
its future effervescent properties.
About the third week in December the wine is racked and
fined and then blended (cuvee) in large vats of about 12,000
gallons capacity. An agitating device worked by hand insures
proper mixing of the wines. The proportions of the blend are
never irrevocably standardized but about 80 per cent by volume
of black grape wine to 20 per cent of white grape wine is aver-
age practice. The vintages of Bouzy and Verzenay are supposed
to impart body and vinosity; those of Ay and Dizy softness and
roundness; and those of Avize and Cramont lightness, delicacy
and effervescence. Some blenders prefer a one-third mixture of
vintages of Sillery, Verzenay and Bouzy, one-third of Mareuil,
Ay and Dizy, and one-third Pierry, Cramont and Avize. Others
advocate an equal mixture of Ay, Pierry and Cramont.
At this stage the important question arises of how much
present and potential carbonic acid gas the wine contains. If it
is too high in sugar and gas, there will be trouble because many
will be lost after the bottling by explosive shattering of the
182
WINE
-
i
= b
a,
E
-
c
u-
CHAMPAGNE 183
bottles and the cellars will be flooded. On the other hand, if
sugar and gas are low the wine will not sparkle properly and
the corks will refuse to pop.
The cuvee is, therefore, tested by means of a glucometer for
sugar and if it registers low the addition is made up by sugar-
candy. If it is high it is necessary to re-ferment it in a cask until
it reaches the right condition.
The cuvee is now fined with isinglass and some tannin is added
to offset ropiness and other defects. It is casked and allowed
to rest for a month. If by that time it has not become clear and
limpid, it is racked off, re-fined and allowed another month to
settle. In some of the largest establishments, mechanical fining
or filtration is now used.
The cuvee is put into new bottles (tirage) . These are usually
new, very strong, and weigh about 2 Ibs. apiece. The pressure
developed by the wine is such that the bottle is always weakened.
It is, therefore, made of special glass which cannot liberate any
alkali to act upon the wine and spoil it.
The tirage is accomplished by running the wine into vats
from which it flows into oblong tanks provided with a row of
syphon taps, at which the bottles are filled. The taps automati-
cally close and stop the flow as soon as the bottle is full.
Next, a culture of selected pure yeast is often added and
the bottles are corked, the corks secured by an iron clip (agrafe)
and the pressure within the bottle determined by an instrument
consisting of a sort of pressure gauge fitted with a hollow screw
at the base. The screw is driven through the cork and the pres-
sure in atmospheres registers on the gauge. A "grand mous-
seaux" represents a satisfactory wine. It has a pressure of 5 3/4
atmospheres and can safely be stored away in one of the cold
subterranean caverns. If the pressure is about 4 atmospheres it
is advisable to store the wine above ground until fermentation
raises its pressure. If the pressure is less than 4 atmospheres it
is advisable to put the wine back in a cask, add cane sugar and
ferment further.
The temperature of the cavern is about 50 F., and must
be kept as constant as possible to avoid too great changes in
WINE
CHAMPAGNE
185
pressure and the bottles bursting in consequence. This is always
a most anxious time. The bottles are placed in preliminary stacks
until this danger is passed and then they are placed in secondary
stacks. Both stackings are arranged horizontally so that the
sediment can work towards the neck of the bottle. The bottles
are even marked with chalk so that the one side remains up-
wards. The duration of the bottle fermentation ranges from
six months to two years.
FIG. 43. Turning champagne bottles. (From Vizetelly, The History of Champagne,
Henry Sotheran & Co., London.)
At the end of that time the bottles are placed in a slanting
position on special stands, with neck tilted slightly down. The
purpose is to induce the sediment to collect on the lower side of
the bottle and to travel towards the neck. A short shaking and
turning movement is given each bottle once each day for six
weeks while the neck is gradually inclined further downwards
until finally the bottle is vertical with the neck pointing straight
down. The shaking and turning of the bottles require great skill
but in spite of this the men develop tremendous speed and handle
incredible numbers per day. The use of a proper variety of
yeast aids tremendously in the settling which is the object of this
part of the process.
i86
WINE
o r
c
'N
"c.3
II
S E
a
CIDER 187
The bottles are now taken to the uncorking room and chilled
to fix the carbon dioxide more firmly. Uncorking is an art. The
workman holds the bottle in a slanting position and gradually
loosens the cork until it together with the sediment is blown out
by the pressure. A finger is inserted to scoop out any remaining
sediment and to stop the wine flowing out. Large establishments
freeze the neck of the bottle and disgorge the sediment in a semi-
solid form. At the same time the bottle is turned upright and
temporarily closed. The champagne is then dosed by adding a
wine solution of sugar and possibly also some brandy and the
bottle is permanently corked. A skilled operator now takes the
bottles and swings them above his head Indian club fashion, which
operation thoroughly distributes the sugar solution throughout
the wine. The bottles are then aged for some time in order to
develop and blend the taste further and to bind the carbon
dioxide.
Imitation Champagne. This is made by carbonating white
wine, or even cider, under pressure in the same manner that soda
water is made. The gas which is forced into solution by this
process never is as firmly absorbed as is the natural carbon dioxide
in true champagne. Hence the wine very quickly loses its sparkle
and becomes flat and lifeless. Nevertheless these imitations are
sold in large volume at considerably lower prices than the genuine
goods since they can be made without either the losses by explo-
sion, etc., the high labor cost, or the long storage of true cham-
pagne. The processing, however, is rather a branch of the car-
bonated beverage industry than of the wine industry. A stricter
interpretation of the term u Imitation Champagne" is sometimes
used which confines it to sparkling wines made by the champagne
process but outside the French Champagne District.
CIDER
This term, in the United States, has generally been applied to
the beverage produced from the unfermented juice of apples.
As such, it is conceded that its consumption exceeds that of any
other beverage juice. However, most farmers permit the cider
which they make for their own use to ferment or become "hard."
i88 WINE
Abroad the word "cider" is applied directly to the fermented
product. The juice of the ripe apples from which cider is made
contain from 7-15% of sugar, the average being around 11%.
Hence the cider, if completely fermented can contain from 3.5-
7.5% of alcohol, and the average product has about 5.5%.
The factors which affect the quality of the finished cider are,
in general, the same as those which affect wine, namely: variety
of fruit, quality of fruit, degree of maturity of fruit, and the
organisms and temperature of fermentation. To make good
cider, first quality, clean apples of a suitable variety, grown espe-
cially for cider making, must be selected. There are possibly as
many varieties of apples as there are of grapes, if not more. The
most important American varieties from their cider making pos-
sibilities are :
Sweet, sub-acid:
Baldwin, Esopus, Hubbardston, Fameuse, Mackintosh, Northwest-
ern, Rome Beauty, and Stark.
Acid:
Winesap, Jonathan, Yellow Newton, Stayman, Northern Spy, and
York Imperial.
Aromatic:
Delicious, Golden Delicious, Lady, Black Gilliflower, White Pear-
man, and Bana Bonum.
Astringent:
Florence, Hibernal, Soulard, Red Siberian, Hyslop, Transcendent,
Launette, Martha, and Yellow Siberian.
Neutral:
Ben Davis, Black Ben, Jana, Willowturg, Missouri, Alexander,
Wolf River, Buckingham, and Limberturg.
In the absence of any of the above varieties, which are called
"vintage apples/' any variety of winter apples is preferable to a
summer variety. With the single exception of winesap apples,
all the others are improved by suitable blending of varieties so
that the desired qualities of flavor, acidity, sweetness, and astrin-
gency are brought to a balance.
The selected fruits are washed, if not already clean, rasped
CIDER 189
to a pulp, rather than crushed, and the pulp is pressed. The
yield of juice varies with the apples and the type of pressing equip-
ment used from 2-4 gallons per bushel. The juice is run into
barrels or vats and either allowed to ferment naturally, or seeded
with a pure culture of wine yeast at the rate of one pint of culture
per fifty gallons of juice. The fermentation must proceed at an
even lower temperature than that of wine, namely 5O-6o F. in
order to avoid injury to the product. The fermentation proceeds
in the usual violent manner, an abundant foam of yeast cells, pec-
tins and albuminoids rising over the liquid as the reaction goes
on. Then when most of the sugar of the must has been exhausted,
in about a month, the foam subsides and the insoluble materials
which it carried settle to the bottom of the barrel. At this time
the batch is racked in a manner similar to wine (see p. 170) and
allowed to carry on a quiet second fermentation at a lower tem-
perature, ca. 45-5O F. This second fermentation requires from
three to six months and should not be entirely complete even
then. Hence, if the cider is racked and bottled at this stage it
will carry on a little further fermentation in the bottle, producing
a beverage with some of the sparkle and life of champagne. A
cider made with care, in the manner described, will be sound and
stable, and unlikely to acetify (turn to vinegar) . It may happen,
however, that some clarification is needed. Formerly, skim milk
in the proportion of one quart to about fifty gallons of cider
was the preferred method of fining. Nowadays modern filtering
equipment with such assistants as purified diatomaceous earth
(kieselguhr) is used.
CHAPTER XII
LIQUEURS AND CORDIALS
General Statement. Liqueurs and Cordials constitute a
group of alcoholic beverages of a somewhat exotic nature. They
are usually made from rectified alcohol, refined cane sugar and
flavoring and aromatic substances extracted from fruits, herbs,
seeds and roots. On account of their high content of sugar they
are rarely consumed in any quantity and serve either as appetizers
or as after dinner relishes.
Liqueurs as a class are very largely of foreign origin and
manufacture and their terminology is somewhat confusing. In
this country the names "liqueur" and "cordial" are practically
interchangeable. Abroad, liqueurs generally are products made
on the continent and especially in France, while cordials are prod-
ucts originating in the United Kingdom or elsewhere. Another
possible distinction is that the liqueurs as a group are more per-
fume-like in character and exclude the cordials which are made
with sharper flavors such as caraway, etc.
Classification. The aim of all cordial and liqueur manufac-
ture is a product in which the various separate constituents are
so blended and united that only a summation is tasted by the
drinker rather than a number of discordant single flavors. The
varying degrees of success with which this object has been
achieved and also the variations in concentration of the liqueur
in alcohol, flavor and sugar have resulted in the recognition, es-
pecially in France, of a number of grades of liqueur, as follows:
1. Ordinaires i. Average
a. Ordinaires a. Single Strength
b. Liqueurs doubles b. Double Strength
2. Demi-fines 2. Good
3. Fine 3. Very good
4. Superfine 4. Excellent
190
MANUFACTURE 191
These grades are independent of the process of manufacture al-
though it may be stated that the highest grades as to smoothness
of flavor can in general only be made by the distillation process.
Manufacture. There are three general methods by which
cordials can be made:
1. The distillation process.
2. The infusion process.
3. The essence process.
In brief statement, the distillation process consists in macerating
the selected aromatic flavoring substances in alcohol for a fixed
period. The liquid is then distilled and the aroma and flavor of
the herbs, seeds, fruits, etc., will be found in the distillate. This
is then sweetened and colored and may also be diluted and blended
with alcohol and water, and other materials as required.
Certain aromas and flavors do not lend themselves to ex-
traction by distillation and in these cases the infusion method is
resorted to. In this process the aromatic substances are steeped
in a solution of alcohol and sugar to which they impart their flavor-
ing and aromatic principles. The solution may be colored and is
then strained to separate the marc or solid residue.
The "liqueurs par infusion" do not have the fine bouquet,
flavor and taste found in the "liqueurs par distillation" with the
exception of infusions of red fruits. These form a group of very
fine liqueurs when they are made according to the best methods
of the art. Typical of the finest are Cherry Brandy, Guignolet
(brandy from black cherries) and Cassis (brandy from black
currants).
In the essence process, essential oils, either natural or syn-
thetic, are added to the alcohol, which is then sweetened and
colored. This kind of liqueur is generally of inferior quality as
compared with the others and should only be made under excep-
tional circumstances or when a cheap product is required.
Whatever general type of manufacture is selected, a special
art is required to produce fine quality products. A series of opera-
tions are involved which must be conducted with skill, care, intel-
ligence and knowledge because the characteristics of the finished
product depend very largely on the technique of preparation,
192 LIQUEURS AND CORDIALS
independent of the variation in quality of the raw materials. This
last is a difficulty which always confronts the liqueur manufac-
turer. No standard formula can be relied on to produce a liqueur
of unvarying quality for the reason that the herbs or seed, etc.,
which flavor it may not have grown under like conditions, or have
ripened equally, etc.
The series of operations involved in the preparation of
liqueurs may include most or all of the following:
Infusion (Maceration)
Distillation
Blending
Coloring
Clarification
Filtration
Aging (True or Accelerated)
Infusion is the process by which the flavoring ingredients are
extracted from their natural raw materials and brought into solu-
tion in the alcohol-water mixture desired. The details of the
process depend very largely on the material which is being ex-
tracted. The strength of the alcohol used may vary according to
the solubility of the flavor in diluted alcohol and also according
to the solubility of such undesired materials as resins, bitter prin-
ciples, etc., which may be present in the herbs. Similar considera-
tions dictate in each special case whether the extraction shall be
performed hot or cold or whether it shall be carried on for days
or only a few hours.
Distillation for liqueur purposes is usually on a small scale
employing a pot still, which, however, in the most modern practice
may be equipped with a reflux condenser to permit partial extrac-
tion at a boil. Whenever extraction is carried on in the still it
is desirable that the latter be equipped with a steam or hot water
jacket to avoid the possibility of burning as by direct heat.
Blending includes the addition of sweetening, and coloring
matters, other flavors, smoothening and softening agents, etc.,
to the distilled flavored alcohol. In France it is very often car-
ried out in a hermetically sealed cylindrical copper vessel called
a conge, see Fig. 45.
MANUFACTURE 193
Note that it is fitted with a sight-glass; i.e., there is an open-
ing about three inches wide running down the side of the vessel
and in this opening is a glass on which is etched a scale marked
off in liters. By means of this sight-glass it is possible to deter-
mine the exact proportions of alcohol, syrup and water in the
conge and also to observe what is happening to them.
Filling, mixing and emptying are all done by hand in the small
establishments. Where the output is greater, the tanks contain-
ing the ingredients are connected to the blending machines by
piping and the feed is under air pressure so that it is only neces-
sary to open each valve for the liquid to run into the blender.
While this takes place the operator reads the quantity on the
sight-glass. Stirring is usually by means of a mechanical agitator
although sometimes it is accomplished manually.
Perfect blending requires the mixing together of the various
ingredients until they form an intimate and homogeneous whole.
In carrying out this operation the following rules will prove of
value:
1 i ) Always add the sugar in the form of a syrup. It is better to
prepare the syrup by dissolving the sugar in hot water, rather than
cold water, as this seems to favor intimate mixing and results in a
liqueur of finer quality and smoothness.
(2) Always blend cold so as to avoid any evaporatio/i of alcohol and
aromatics and to prevent any spoilage which may ensue.
(3) Observe one of the following orders of addition: (a) put the
aromatic spirit in first, (b) add the extra alcohol and stir for about
ten minutes, (c) add the syrup and stir again, (d) add the re-
quired quantity of water and stir again in order to thoroughly
incorporate the various ingredients. Some liqueur manufacturers
favor a reverse order of procedure: (a) water, (b) sugar and
glucose, (c) alcohol and alcoholic tinctures, (d) aromatic spirits,
etc. Once the blending has been completed the coloring is added
and stirred in.
The liqueur is allowed to rest for two or three days after
mixing in order to give the ingredients time to blend thoroughly
together. Thereafter, it is sampled to determine whether it has
the desired combination of characteristics. If it is unsatisfactory.
194 LIQUEURS AND CORDIALS
the operator must make such additions and modifications as his
experience suggests.
In the United States especially and also in many places abroad
it has been found that the use of a closed blending tank is not
essential, particularly for the spicier liqueurs sometimes classed
as cordials. An open, copper-lined tank is used and agitation
supplied either mechanically or manually. The order of addition
of the ingredients remains important, however. This probably
derives its weight partly from the necessity of preventing the
precipitation of alcohol-soluble flavors from a strong solution by
too great dilution with water; and partly to allow the escape of
air dislodged from solution before the flavors are attacked and
oxidized. Whatever method of blending is followed the finer
liqueurs require aging to unite their constituents firmly in a per-
fect blend and give them smoothness.
Aging of liqueurs depends only slightly on chemical reaction,
but more on the effect of time to cause the desired union of flavors.
Hence it may very well take place either in bottles or casks. The
time required is seldom more than a few days to a few months.
As with all changes in which time is involved, the elevation of
temperature causes acceleration of the change. Hence, in the
home of liqueurs, France, a special technique has been developed
and given a name, "Tranchage" for the accelerated aging of
liqueurs. The process is not universally applicable since it causes
rancidity in some liqueurs, e.g., anisette and creme de menthe. It
also spoils chartreuse whose volatile oils will only commingle with
time rather than heat. With care, however, it is an excellent and
much used method.
Tranchage is accomplished by heating the liqueur gradually
to a temperature of 70 to 90 C. in a hermetically sealed vessel.
Heat is supplied either by a water or a steam jacket. When the
set temperature has been reached the heating medium is with-
drawn and the liqueur allowed to cool slowly.
The treatment is usually given in an apparatus called a "conge
a trancher" see Fig. 45. This vessel is fitted with a safety valve,
a thermometer, a sight-glass and a steam coil, and is the type
mostly used in medium sized plants. The larger manufacturers
MANUFACTURE
195
use a cylindrical tank fitted with legs, a large, quick-closing man-
hole on top and a safety valve, and an inlet tap for the compressed
air. Below is an exhaust valve for the air.
The usual sight-glass with scale graduated in litres is
on the side. The bottom is fitted with valves for drawing off
the liqueur, either by gravity into jugs or under pressure. There
FIG. 45. Liqueur blending equipment (conge a trancher).
is a separate tap for drawing off wash water. A steam coil is
provided for heating and a mechanical agitator for mixing.
The method of operation is as follows: The feed taps for
the ingredients are opened successively and the required quanti-
ties of each liquid are run in. Then the contents of the vessel
are agitated. When blending is completed the steam valve is
opened and the mixture is heated until the temperature reaches
196 LIQUEURS AND CORDIALS
the maximum allowable. Then the liqueur is either run off into
casks under air pressure or is allowed to rest in the conge, whence
it is run off, colored, filtered, and either barrelled or bottled.
Coloring of liqueurs is done to add what the jargon of the
advertising profession calls "eye appeal' 1 to the liqueur. Unless
it is done with knowledge of the properties of the color used it is
a risky business. On occasion the stronger colors may alter the
taste and break up the harmonious blend of aromatics in the
liqueur. Again the colors may be affected by light in storage
and bleach or precipitate in the bottle. Infusions of red fruit
tend to bleach to pinks and the violet ones tend to darken. The
yellows tend to turn brown. Many of these changes can be
averted by suitable skill or by proper selection of colors. Above
all, where artficial aging is used, it is desirable to add color after
the liqueur has cooled so that the effect of heat on the color will
be avoided. With some vegetable colors the addition of about
0.01-0.02% of alum to the liqueur is claimed to give permanence
and stability.
Clarification or fining of liqueurs is practiced not only to give
them limpidity and brilliancy so that they are agreeable to the
eye, but also to render them immune against changes caused by
substances which they may hold in suspension.
Clarification methods precipitate these insoluble substances so
that they can be removed by filtration. Both these operations are
preferably carried out after the liqueur has completely cooled
following tranchage, or better still after resting and settling for
several days.
Various substances are used: albumen, white of egg, fish glue,
gelatin, and skimmed milk, or the modern filter aids such as talc,
asbestos, kieselguhr, etc.
Sample procedures: To fine one hectoliter (25 gals.) of
liqueur are as follows:
Take three whites of egg and whip them up in a liter (quart) of water;
pour it into the liqueur; stirring all the time; allow it to rest and settle
for 24 to 48 hours ; then decant.
Fining by means of white of egg works very well with cloudy
MANUFACTURE 197
or milky liqueurs. It also works well with liqueurs made by the
infusion process, but in this case only one white of egg must be
used to avoid altering the coloring material, which is partially
precipitated by the albumen.
Fish glue or isinglass is more often used. It works very well
with strongly alcoholic liqueurs but its preparation is somewhat
lengthy and calls for considerable care.
The best method of procedure is as follows:
Macerate the fish glue for 24 hours in ten times its weight of water,
taking care to renew the water two or three times because the glue will
otherwise putrefy and acquire a nauseating odor. When the glue becomes
soft, wet, and white, it is put into a mortar and pounded for some time
so as to disintegrate it and separate all fibres. In this condition, small
quantities of fresh water are added to it gradually, with stirring until a
milky suspension or solution results. This liquid is strained through silk
or fine linen cloth. The coarse undisintegrated particles of glue left upon
the silk or linen strainer are put back into the mortar and pounded again.
Water is then added in the same manner as before and the whole pro-
cedure is gone through again until very little residue remains. The sus-
pension is now stirred vigorously and a solution of tartaric acid is added,
the stirring is continued until the glue goes into solution.
The final product is not a white, limpid, easily flowing liquid but
a kind of thin, transparent jelly which should be free of every
trace of animal fiber. The materials should be used in about the
following proportions :
Fish glue 10 grams y$ oz.
Tartaric acid (dissolved in half a liter of
water i pt. ) r gram 1 5 gr.
i to 1^/2 liters
Water I i to iy 2 quarts
for one hectoliter (25 gals.) of liqueur. The jelly solution is
poured into the liqueur which is then well stirred up and finally
allowed to rest for two or three days.
Another method replaces water as a solvent by either white
wine or water to which some vinegar has been added. In this
case it is not necessary to add tartaric acid. Ten per cent of alco-
hol added to the dissolved fish glue will preserve it from putrefy-
198 LIQUEURS AND CORDIALS
ing in the event that the glue solution is made up for some time
before using.
To fine with gelatin soften 30 grams (i oz.) in a liter (i
quart) of warm water; add the mixture to the liqueur; stir in
vigorously and allow to rest for several days. This type of
clarification agent is best adapted for white liqueurs of low alcohol
content.
Milk is also a good clarification agent for white liqueurs of
low alcohol content. It should be added in the proportions of
one liter (i quart) of milk to each hectoliter (25 gals.) of
liqueur. It is advisable to boil the milk and the liqueur should
be well stirred while the addition is made. Milk makes a par-
ticularly good fining agent for the curagaos.
Always fine cold because hot fining results in the liqueur ac-
quiring an albuminous taste which is very difficult to eliminate.
Filtration of liqueurs is done in order to give them the final
"polish" that ensures brilliant clarity and absence of turbidity.
The means by which it is accomplished range from a simple felt or
flannel bag to more mechanical filters of larger capacity. In any
type of filter the true filtration is done by some powdered material
added to the liqueur which builds up a cake on the meshes of the
filter apparatus and holds back the slimy suspended matter with-
out clogging. Hence it is always necessary to return the first
runnings of the filter one or more times until an efficient coating
of filtering medium has been produced and the filtrate is abso-
lutely clear. The felt bag filter is used in the same manner as the
domestic jelly bag. That is, it is suspended with a hoop to keep
its mouth open and filled with a bucket. It drains into another
bucket. In spite of its primitiveness it is an effective filter for
small lots of material. The next type of apparatus used for
filtration is a copper cone fitted with a faucet at the bottom. To
use this filter close the faucet and line the cone with filter paper
or preferably pack the bottom with pure cellulose or filter paper
reduced to pulp with a little water. The cone is filled with liqueur
and the faucet opened. Figure 46 shows such a cone filter.
Figures 47 and 48 show a slightly more advanced type
of filter and its method of application. It consists of a tinned
MANUFACTURE
199
FIG. 46.
FIG. 47. Wire mesh liqueur FIG. 48. Method of connecting and operating liqueur
filter. filter shown in Fig. 47.
200 LIQUEURS AND CORDIALS
copper cylinder fitted with a faucet at the bottom and valves at
the side and top. The cover seals it hermetically. The interior
consists of two metallic screens, one with horizontal and vertical
shoot and warp wires; the other, a cone, with diagonal shoot and
warp. It is necessary to disperse some kind of filtering material
in the liqueur, so that this material deposits on the screens and
aids in the production of a clear filtrate. Paper pulp, asbestos
wool, talc, diatomaceous earth, etc., are satisfactory for this
purpose. The method of application is shown in Fig. 48. If
necessary, it is possible to arrange the filter and casks in battery
form, so that the receiving barrel of one filter serves as the feed-
ing barrel of another filter.
Similar filters are used in which the capacity is increased by
supporting the wire filter cloth over a thin hollow rectangular
frame and placing a number of these in a container so that the
liquid flows freely into the outer chamber, and after passing
through the filtering surface is collected from the interior of the
frame and drained into a storage vessel.
CURASAO
In order to summarize the actual application of the general
process outline given above, the manufacture of Curasao is de-
tailed here because this liqueur has probably become the one best
acclimated on American soil and is made here in larger volume
than any other. The Curasao fruit is one of the family of bitter
oranges. They grow chiefly in the West Indies and the price for
genuine Curasao peels is quite high so that distillers generally
substitute up to 50% of other bitter orange peels in the cheaper
liqueurs.
Manufacture. The outstanding characteristic of Curasao
liqueurs is a mild bitter taste derived from the maceration of the
fresh Curasao peel in 190 proof alcohol. Very little of this ex-
tract needs to be incorporated into the finished liqueur on account
of its intense bitterness. The complete process of making Cura-
gao liqueur as stated by Wolff (Spirits (1934) II, No. 6, 73)
is as follows :
b.
CURAgAO 201
FORMULA TO MAKE IOO GALLONS
CURACAO TRIPLE SEC. 40% ALCOHOL BY VOLUME
EXTRA FINEST QUALITY
24 oz. Extra thin genuine fresh Curasao peels
12 oz. Extra thin fresh Orange peels
Grind and macerate for 2 days with
2.5 gal. Alcohol 190 proof (95%)
Draw off 2 gallons of Extract. To the remaining macer-
ate add:
20 Ib. Extra thin fresh Curasao peels
15 Ib. Extra thin fresh Orange peels
10 oz. Mace
2 oz. Cloves
38 gal. Alcohol 190 proof
40 gal. Distilled water
Digest for six hours at very gentle heat, place in a steam
jacketed still, add another 5 gallons water, and distill slowly for
2 hours with partial reflux until all the alcohol is driven over.
Rectify the raw distillate to 35% alcohol by volume and filter
clear over Kieselguhr to remove terpenes. Clean still and then
rectify the filtered distillate to 58 gallons, 60% alcohol by
volume.
The extract and distillate are blended as follows :
BLENDING FORMULA
2 gal. Extract a.
58 gal. Rectified distillate 60% b.
1 gal. Genuine Jamaica Rum 74%
4 gal. Grape distillate 60%
2 gal. Port wine
5 gal. Glucose 42 B.
1 8 gal. Syrup made from
250 Ib. best grade sugar
25 Ib. milk sugar
i Ib. Citric Acid C.P.
13 gal. Distilled water
Caramel color as needed.
This formula will vield 100 eallons.
202 LIQUEURS AND CORDIALS
A cheaper product is made as follows :
1.5 Ib. Extra thin Curasao peel
Macerate for two days with 1.5 gal. alcohol and draw off
i gallon extract.
To the remaining macerate add:
2O Ib. Extra thin Curasao peel
10 Ib. Dried expulped Curasao peel
10 oz. Mace
2.5 oz. Cinnamon
2.5 oz. Cloves
13 gal. Alcohol 190 proof (95% vol.)
15 gal. Distilled water
Direction for distillation same as preceding formula except
that 20 gallons of rectified distillate at 60% are obtained.
BLENDING FORMULA
1 gal. Extract a'.
20 gal. Rectified distillate 60% b'.
0.5 gal. Genuine Jamaica Rum 74%
2.5 gal. Grape distillate 60%
24.5 gal. Alcohol 1 90 proof (95%)
2 gal. Port wine
23 gal. Syrup made from
300 Ib. sugar
20 Ib. milk sugar
I Ib. Citric acid C.P.
29.5 gal. Distilled water
Caramel color as needed.
Newly made Curasao liqueurs have a raw unpleasant taste of peel
which the addition of milk sugar helps to overcome. Heating the liqueur
in vacuo to 135 F. also accelerates aging the product.
LIQUEUR FORMULAE
There follows a selected list of formulae for the manufacture
of liqueurs. In the case of many liqueurs a number of alternative
formulae are cited according to the method of manufacture and
the grade or quality of product. In using these formulae, the
warning must be observed that no amount of direction can sub-
stitute safely for care, skill and experience.
In explanation of the following formulae it is also important
to note that the words "spirit of' refer to an alcohol distillate
LIQUEUR FORMULAE 203
from the flavoring material. The term essence refers to a solu-
tion of the essential oil in alcohol. Directions for coloring have
been omitted, as the user will naturally follow his judgment in
this matter. The section on coloring in this chapter and the list
of colors in Chapter IV may be helpful in this connection.
ABSINTHE
First Quality
Wormwood 28 Ib.
Hyssop 6 Ib. 8 oz.
Lemon balm 6 Ib. 8 oz.
Anis (green) 40 Ib.
Chinese aniseed 12 Ib.
Fennel 16 Ib.
Coriander 8 Ib.
Alcohol (90%) , 80 gal.
Water 25 gal.
Macerate for 48 hours. Distill. Color with an infusion of worm-
wood and green herbs.
CREAM OF ABSINTHE
First Quality "Synthetic"
Essence of absinthe 45 min.
" " English peppermint 45 min.
" " anis 4 dr.
' ' " sweet fennel i dr.
' ' distilled lemon 4 dr.
Alcohol (85%) 4 gal.
Sugar 45 Ib.
Water to make 10 gal.
ABSINTHE
Average Quality
Essence of absinthe 45 min.
' ' ' * English peppermint 45 min.
' ' ' * anis, green 4 dr.
" " lemon 4 dr.
" ," fennel I dr.
Alcohol (85%) 2. 5 gal.
Sugar 10 Ib.
Water to make 10 gal.
204 LIQUEURS AND CORDIALS
ALKERMES DE FLORENCE
Elixir of Life of Florence
Essence of calamus 22 min.
' * ' ' Chinese cinnamon 15 min.
" * * cloves. . 40 min.
* * ' ' nutmeg 22 min.
' ' ' ' roses 30 min.
Extract of jasmin 4 dr.
" " anis 4 dr.
Alcohol (85%) 4 gal.
Sugar 45 Ib.
Water to make 10 gal.
Color with cochineal
ANGELICA LIQUEUR
Excellent Quality
Angelica root 10 Ib.
seed 8 Ib.
Coriander seed i Ib.
Fennel i Ib.
Alcohol (90%) 28 gal.
Macerate, distill and rectify to 36 gallons after addition of water. Add
400 Ib. of sugar in syrup and make to 100 gallons with distilled water.
Very Good Grade
Spirit of angelica root 10 gal.
11 " " seeds 10 gal.
Alcohol (85%) 13.5 gal.
Sugar 342 Ib.
Water to make 100 gal.
Good Grade
Spirit of angelica roots 2 qt. 25 oz.
' ' ' ' ' ' seeds 2 qt. 25 oz.
Alcohol (85%) i gal. 3 pt.
Sugar 20 Ib.
Water to make 10 gal.
Average Grade Double Strength
Spirit of Angelica seeds i gal. 3 pt.
Alcohol (85%) 3 gal. 5 pt.
Sugar 20 Ib.
Water to make 10 gal.
LIQUEUR FORMULAE 205
Average Grade Single Strength
Spirit of angelica seeds 3 qt. 12 oz.
Alcohol (85%) i gal. 6 pt.
Sugar 10 Ib.
Water to make 10 gal.
ANISETTE
Highest Quality Paris Type
Chinese aniseed 16 Ib.
Bitter almonds 4 Ib.
Green anis 16 Ib.
Coriander 2 Ib.
Fennel i Ib.
Angelica roots 4 oz.
Lemon peel No. 80
Orange peel No. 80
Alcohol (90%) 34 gal.
Macerate in alcohol for 24 hours, add 19 gallons of water, distill. Add
19 gallons of water and rectify to draw off 36 gallons of good product.
Dissolve 400 Ib. of refined sugar in 24 gallons of water and cool. Add
this to the distillate and add:
Infusion of orris 4 oz.
Orange flower water i gal.
Chinese aniseed water 8 oz.
Clove water i .5 oz.
Nutmeg water 1.5 oz.
Add enough water to make up to 100 gallons.
Alternative
Anis de Tours 8 Ib.
Anis d'Albi 8 Ib.
Badiane (Chinese Aniseed) 4 Ib.
Ceylon cinnamon i Ib.
Orris 12 oz.
Cloves 3 oz.
Angelica root 3 oz.
Dictame de Crete (marjoram) 12 oz.
Coriander seed 12 oz.
Almonds (sweet) 4 Ib.
206 LIQUEURS AND CORDIALS
Lemon peels No. 80
Orange peels No. 20
Nutmegs No. 40
Alcohol (85%) 40 gal.
Macerate for 24 hours, add water, distill, rectify, sweeten to 45.
Add I gallon of orange flower oil.
Anisette Bordeaux Type
Badiane (Chinese aniseed) seeds 16 Ib.
Anise (green) 4 Ib.
Fennel 4 Ib.
Coriander 4 Ib.
Sassafras 4 Ib.
Musk seed 14 oz.
Lemon peel 4 Ib.
Alcohol (90%) 35 gal.
Macerate for 48 hours in alcohol. Add 30 to 40 gallons of water.
Distill. Add 35 gallons of alcohol and 20 gallons of water and rectify.
Dissolve 400-500 Ib. of sugar in hot water. Mix the syrup with the
alcohol. This should give a total volume of 100 gallons. Filter. Add
I or 2 gallons of orange flower oil.
Very Good Grade
Spirit of anise (prepared as above) 2.5 gal.
Orange flower water I pt.
Infusion of orris 3 oz.
Alcohol (85%) 3 gal.
Sugar 1 9 Ib.
Water to make 10 gal.
Good Grade
Spirit of anise 3 qt.
Orange flower water 12 oz.
Alcohol (85%) 2.5 gal.
Sugar 20 Ib.
Water to make 10 gal.
These liqueurs should be colored red.
LIQUEUR FORMULAE 207
Anisette (with Glucose)
Spirit of anise 3 qt.
Orange flower water 3 qt.
Alcohol (90%) 1.75 gal.
Sugar 10 Ib.
Glucose (36 B) 2.75 gal.
Water to make 10 gal.
Average Grade Double Strength
Spirit of anise 3.5 qt.
Alcohol (85%) 4.25 gal.
Sugar 20 Ib.
Water to make 10 gal.
With Glucose
Spirit of anise 3.5 qt.
Alcohol (90%) 1.5 gal.
Sugar 12 Ib.
Glucose (36 B) 3.75 gal.
Water to make 10 gal.
Single Strength
Spirit of anise 0.5 gal.
Alcohol (85%) 2 gal.
Sugar 10 Ib.
Water to make 10 gal.
With Glucose
Spirit of anise 0.5 gal.
Alcohol (90%) 2 gal.
Sugar 5 Ib.
Glucose (36 B) 1.75 gal.
Water to make 100 gal.
" SYNTHETIC "ANISETTE
Highest Grade
Essence of Chinese aniseed i oz.
" , " anise 2 dr.
" " sweet fennel i dr.
" " coriander 5 min.
" "sassafras 45
208 LIQUEURS AND CORDIALS
Extract of orris 0.75 oz.
" " amber (not musk) i dr.
Alcohol (85%) 4 gal.
Sugar 45 Ib.
Water to make 10 gal.
Very Good Grade
Essence of Chinese aniseed 6 dr.
" " anise 2 dr.
sweet fennel 45 min.
" " coriander 5 min.
sassafras 30 min.
Extract of orris 4 dr.
" " amber (not musk) 45 min.
Alcohol (85%) 3- 2 5g*l.
Sugar 30 Ib.
Water to make 10 gal.
Ordinary Grade
Essence of aniseed 3 dr.
" Chinese aniseed 3 dr.
' ' * ' sweet fennel 40 min.
* ' ' ' coriander 4 min.
Alcohol (85%) 2.5 gal.
Sugar 10 Ib.
Water to make 10 gal.
Benedictine
This product is made only by a company once the Benedictine Monks
of Fecamp. Through hundreds of years they have kept its composition
secret and have now a copyright on the name and bottle. The formula
cited is an imitation which closely reproduces the original.
Cloves 4 oz.
Nutmeg I oz.
Cinnamon \ oz.
Mixture of peppermint, fresh angelica roots and
alpine mugwort 3^ oz.
Aromatic calamus 2 oz.
Cardamom, minor 7 oz.
Flowers of arnica i oz.
Cut up and crush the materials and macerate for two days
LIQUEUR FORMULAE 209
in 4 gallons of 85 per cent alcohol. Add 3 gallons of water and
draw off 4 gallons. Distill. Add syrup made with 32 Ib. of
sugar and 2 gallons of water. Make the volume up to 10 gal-
lons. Color yellow and filter.
BLACK CURRANT BRANDY (LIQUEUR)
(Creme de Cassis)
Excellent Quality
Infusion of black currants (first) 4 gal. i qt.
Spirit of strawberries 2 qt.
Alcohol (85%) 2 qt. i pt.
Sugar, 40 Ib.
Water to make 10 gal.
In the formula just cited, as well as in the next following
formulae reference is made to different infusions. To prepare
these infusions the following directions are given: Steep or mace-
rate the fruits or other flavoring ingredients in alcohol. When
extraction appears complete, decant the solvent and use as the
first infusion. A second and third infusion may be made from
the same fruits but on account of the comparative weakness of
these in extract they must be employed in the ratios of i : 2 and
i : 3 to replace a first infusion. In balancing the formula correc-
tion must be made in the amount of neutral spirits added to com-
pensate for the alcoholic content of the volume of infusion used.
Very Good Grade
(Ratafia de Cassis)
Infusion of black currants (first) 3 gal. 5 pt.
" " strawberries 3 qt. 12 oz.
Alcohol (85%) i gal
Sugar 30 Ib.
Water to make 10 gal.
Good Grade
Infusion of black currants (first) 2 gal. 3 pt.
Vin de Roussillon 3 qt. 12 oz.
Infusion of wild cherries 3 pt.
* * ' ' strawberries 3 pt.
Alcohol (85%) 2 gal. 3 qt.
Sugar 20 Ib.
"Water to make total volume up to 10 gallons.
210 LIQUEURS AND CORDIALS
Average Grade Double Strength
Infusion of black currants (first) 2 gal.
Alcohol (85%) 2 gal. 3 pt.
Sugar 20 Ib.
Water to make 10 gal.
Average Grade Single Strength
Infusion of black currants i gal. 2 qt.
Alcohol (85%) i gal. i qt.
Sugar 10 Ib.
Water to make 10 gal.
CREAM OF CELERY
(Crime de Celeri)
Very Good Grade
Spirit of celery 2 gal.
Alcohol (85%) i gal. I qt.
Sugar 35 Ib.
Water to make 10 gal.
Good Grade
Spirit of celery i gal. i qt.
Alcohol (85%) i gal. 5 pt.
Sugar 20 Ib.
Water to make 10 gal.
Good Grade "Synthetic"
Essence of celery 2 dr.
Alcohol (85%) 3 gal- i Pt.
Sugar 35 lb -
Water to make 10 gal.
CHARTREUSE
See remarks under Benedictine
Green Chartreuse
Melisse citronne, dry (lemon balm) 8 Ib.
Hyssop flowers 2, Ib.
Dry peppermint 2 Ib.
Alpine mugwort 2 Ib.
Balsamite x Ib.
Thyme 7 oz
LIQUEUR FORMULAE 211
Angelica leaves i Ib. 5 oz.
' ' roots i Ib. 5 oz.
Arnica flowers 3 oz.
Bourgeons de peuplier-baumier 3 oz.
Chinese aniseed 2 oz.
Mace 2 oz.
Alcohol (90%) 58^ gal.
Macerate for 24 hours, add water and rectify to draw off 60 gallons;
add sugar syrup made by dissolving 200 Ib. of sugar in hot water, mix and
make total volume up to 100 gallons with water; age by heating; then
color green with blue color and saffron or caramel, according to the de-
sired shade.
Rest, fine and filter.
Yellow Chartreuse
Lemon balm 4 Ib.
Hyssop flowers i Ib.
Alpine mugwort i Ib.
Angelica leaves 2 Ib.
* ' roots 2 Ib.
Arnica flowers 2 oz.
Chinese aniseed 2 oz.
Mace 2 oz.
Coriander 12 Ib.
Aloes 4 oz.
Cardamom, minor 4 oz.
Cloves 3! oz.
Alcohol (90%) 38 J gal.
Refined sugar 200 Ib.
Water, to make up to 100 gallons.
Proceed as above, coloring yellow with saffron.
White Chartreuse
Lemon balm 4 Ib.
Hyssop flowers i Ib.
Alpine mugwort i Ib.
Angelica leaves 2 Ib.
' ' roots 13 oz.
Chinese aniseed 13 oz.
Mace 4 oz.
Cloves 4 oz.
2i2 LIQUEURS AND CORDIALS
Nutmeg 4 oz.
Cardamom, minor 4 oz.
Calamus, aromatic 4 oz.
Tonka beans i J oz.
Alcohol (90%) 49 gal.
Refined sugar 300 Ib.
Water to make up to 100 gallons.
Prepare as above.
The monks age their product for two or three years.
First Quality "Synthetic"
Essence of lemon 15 min.
' ' ' ' hyssop 15 min.
' ' ' ' angelica I dr.
" " English peppermint 2 dr.
* ' " chinese aniseed 15 min.
1 ' ' * nutmeg 15 min.
' * * * cloves 15 min.
Alcohol (85%) 4 gal.
Sugar 45 Ib.
Water to make 10 gal.
Color: yellow or green.
CHERRY CORDIAL
(Ratafia de cerises de Grenoble)
First Quality , Grenoble Type
Infusion of cherries 2^ gal.
* ' ' ' wild cherries i \ gal.
Spirit of apricot stones 5 pt.
* * ' ' strawberries 3 pt.
Sugar 40 Ib.
Water to make 10 gal.
Angers' Type
Guignolet d* Angers
Infusion of cherries 2 gal.
" ' * wild cherries 2 gal.
Alcohol (85%) i gal.
Sugar 40 Ib.
Water to make 10 gal.
LIQUEUR FORMULAE 213
Very Good Grade
Infusion of cherries 3 J gal.
" " wild cherries 3 qt. 12 oz.
Spirit of apricot stones 3 qt.
Alcohol (85%) i qt. 22 oz.
Sugar 30 Ib.
Water to make 10 gal.
Good Grade
Infusion of cherries. 3 gal.
" ' ' wild cherries 2 qt.
Spirit of apricot stones 2 qt.
Alcohol (85%) i qt. 22 oz.
Sugar 20 Ib.
Water to make 10 gal.
CREAM OF COCOA
(Creme de Cacao)
Highest Quality
Cocoa (Caracas) 20 Ib.
Cocoa (maragnan) 20 Ib.
Cloves 7 oz.
Mace 8 oz.
Vanilla. 4 oz.
Alcohol (85%) 40 gal.
Roast the cocoa, grind it. Macerate in alcohol the cocoa, cloves, mace,
and vanilla and distill after 48 hours. Rectify. Add i gallon of tincture
of vanilla and 400 Ib. of refined sugar which has been dissolved in a suffi-
cient quantity of water to bring the total quantity of liqueur to 100 gal-
lons. The tincture of vanilla adds, in addition to flavor, a light yellow
color which is much admired.
CREAM OF COFFEE
(Creme de Moka)
Very Good Grade
Spirit of moka (spirit of coffee) 2j gal.
Alcohol (85%) 6 pt.
Sugar 35 Ib.
Water . . to make 10 gal.
2i 4 LIQUEURS AND CORDIALS
Good Grade
Moka water (aqueous extract of coffee) .... 2 gal.
Alcohol (85%) 2 gal. 6 pt.
Sugar 20 Ib.
Water to make 10 gal.
CURACAO
The best as well as most detailed directions for making
Curasao will be found on p. 201 et seq. in this section. How-
ever, a number of alternative formulae have been included here
to guide in the preparation of different grades of the liqueur. In
each of the formulae cited below the addition of caramel color is
required.
Highest Quality Triple Sec.
Dutch Curasao peel 64 Ib.
Curasao reeds 32 Ib.
Orange peels No. 6
Lemon peels No. 4
Alcohol (85%) 50 gal.
Distill, rectify. Add:
Infusion of oranges 3 gal.
* ' ' * curagao reeds 2 gal.
Sweeten with
White sugar 200 Ib.
Raw white sugar 80 Ib.
Color and filter.
Very Good Grade
Spirit of Dutch Curasao 2| gal.
' ' ' * oranges 3 qt.
Infusion of Curasao 3 oz.
Sugar 35 Ib.
Water to make 10 gal.
Good Grade
Spirit of Curasao i gal i qt.
Infusion of curaf ao 4 oz.
Alcohol (85%) ij gal.
Sugar 20 Ib.
Water to make 10 gal.
LIQUEUR FORMULAE 215
Average Grade Double Strength
Spirit of Curasao i gal.
Alcohol (85%) 4 gal.
Sugar 20 lb.
Water to make 10 gal.
(With Glucose)
Spirit of curagao i gal.
Alcohol (90%) i\ gal.
Sugar 13 lb.
Glucose (36 B) 3 gal 3 qt.
Water to make 10 gal.
Average Grade Single Strength
Spirit of Curasao 3 qt. 12 oz.
Alcohol (85%) i gal. 3 qt.
Sugar 10 lb.
Water to make 10 gal.
Proceed as above and color with a little caramel.
(With Glucose]
Spirit of Curasao 3 qt. 1 2 oz.
Alcohol (90%) i gal. I qt.
Sugar 4! lb.
Glucose (36 B) i gal. 7 pt.
Water to make 10 gal.
Highest Quality "Synthetic"
Essence of distilled Curasao i oz. 2 dr.
" Portugal, distilled 4 dr.
Infusion of bitter Curasao sufficient quantity
Alcohol (85%) 4 gal.
Sugar 45 lb.
Water to make 10 gal.
Very Good Grade " Synthetic "
Essence of distilled Curasao f oz.
" Portugal, distilled 2 dr. 30 min.
" " cloves 30 min.
Infusion of bitter curacao sufficient quantity
Alcohol (85%) 3 gal- i qt.
Sugar 3 6 lb -
Water to make 10 gal.
2i 6 LIQUEURS AND CORDIALS
Average Grade "Synthetic"
Essence of Curasao 4 dr.
" " Portugal, distilled i dr. 30 min.
" " cloves 20 min.
Alcohol (85%) 2j gal.
Sugar 10 Ib.
Water to make 10 gal.
DESSERT LIQUEUR
(Liqueur de Dessert)
Angelica seed 6 Ib.
root 4 Ib.
Calamus (aromatic) i Ib. 4 oz.
Ceylon cinnamon i Ib. 4 oz.
Myrrh 12 oz.
Cloves 10 oz.
Aloes 7 oz.
Vanilla 8 oz.
Nutmegs No. 20
Saffron f oz.
Alcohol (86%) 40 gal.
Crystallized sugar 400 Ib.
Water: sufficient to make up to 100 gal. total volume.
Macerate in alcohol 48 hours. Distill. Rectify, color with tincture
of saffron. Filter.
GARUS* ELIXIR
(Elixir de Gar us)
Spirit of aloes 14 oz.
" " myrrh 14 oz.
" * ' saffron 14 oz.
" " Chinese cinnamon 14 oz.
cloves 8 oz.
nutmeg 7 oz.
Orange flower water 14 oz.
Alcohol (85%) 2 gal. 3 pt.
Sugar 20 Ib.
Water to make 10 gal.
Color golden with saffron and a little caramel.
t < ( i
(I <
LIQUEUR FORMULAE 217
GOLDEN ELIXIR
(Eau de vie de Dantzick)
Ceylon cinnamon 8 Ib.
Ripe figs 8 Ib.
Cumin i Ib. 12 oz.
Musk seed 14 oz.
Mace i Ib.
Cloves i Ib.
Lemon peel i Ib.
Alcohol (86%) 40 gal.
Refined white sugar 392 Ib.
Macerate in alcohol 48 hours. Distill. Rectify. Dissolve sugar in
sufficient water to make total volume up to 100 gallons. Settle. Filter.
Add I leaf of gold per gallon. Agitate and bottle.
HENDAYE'S ELIXIR
(Eau de vie de Hendaye)
Very Good Grade
Spirit of anis i qt.
" ' ' coriander i qt.
' ' ' ' bitter almonds i qt.
' * * * angelica root \ gal.
" " cardamom, major 7 oz.
" " " minor 7 oz.
" " lemon 14 oz.
" ' ' oranges % gal.
Infusion of orris 3 oz.
Alcohol (85%) i J gal.
Sugar 35 Ib.
Water to make 10 gal.
Kirs chw ass er Liqueur
Kirsch, fine (true cherry brandy) (50%).. . . 15 gal.
Spirit of nuts (cherry stone or bitter almond) 10 gal.
Orange flower water i gal.
Alcohol (90%) i$ gal.
Sugar 400 Ib.
Water to make 100 gal.
2i 8 LIQUEURS AND CORDIALS
Huile de Kirschwasser "Synthetic"
Essence of nuts 4 dr.
*' " French neroli oil 40 min.
Alcohol (85%) 4 gal.
Sugar 45 lb.
Water to make 10 gal.
CREME DE MENTHE
Very Good Grade
Spirit of peppermint 2^ gal.
Alcohol (85%) 3 qt.
Sugar 35 lb.
Water to make 10 gal.
Color green with mixture of blue and yellow colors if desired.
Good Grade
Peppermint water i gal.
Alcohol (85%) 2 gal. 3 qt.
Sugar 20 lb.
Water to make 10 gal.
Alternative Formula
Peppermint water i gal. i qt.
Alcohol (85%) 5 gal.
Sugar 20 lb.
Water to make 10 gal.
Average Grade
Peppermint water 3 qt. 12 oz.
Alcohol (85%) 2 gal.
Sugar 10 lb.
Water to make 10 gal.
Very Good Grade "Synthetic"
Essence of English peppermint 5 dr.
Alcohol (85%) 3 gal- J qt-
Sugar 35 lb.
Water to make 10 gal.
LIQUEUR FORMULAE 219
Good Grade "Synthetic"
Essence of English peppermint 3 dr. 30 min.
Alcohol (85%) 2 gal. 3 qt.
Sugar 20 Ib.
Water to make 10 gal.
NUT BREW
(Brou de Noix)
Good Grade
Infusion of nuts 3 gal.
Spirit of nutmeg 5 oz.
Alcohol (85%) \\ gal.
Sugar 30 Ib.
Water to make 10 gal.
Color with caramel.
Average Grade Double Strength
Infusion of nuts 4 gal. I qt.
Spirit of nutmegs 7 oz.
Alcohol (85%) aj gal.
Sugar 20 Ib.
Water to make 10 gal.
Color with caramel.
Average Grade Single Strength
Infusion of nuts, aged 2 gal. i pt.
Spirit of nutmeg 3 oz.
Alcohol (85%) i gal. 3 pt.
Sugar 44 Ib.
Water to make 10 gal.
Color with caramel.
NOYAUX
(Eau de Noyaux)
Finest Quality
Apricot stones 16 Ib.
Cherry stones 12 Ib.
Dried peach leaves 4 Ib.
Myrrh I Ib. 10 oz.
Alcohol (90%) 40 gal.
Water to make 100 gal.
Crush the stones, macerate, add water and distill.
220 LIQUEURS AND CORDIALS
CRME DE NOYAUX
Very Good Quality
Spirit of apricot stone i gal. 5 pt.
" " bitter almonds I pt.
Orange flower water 3 qt.
Alcohol (85%) 3 qt.
Sugar 35 Ib.
Water to make 10 gal.
Good Grade
Spirit of apricot stones i gal. 3 pt.
Alcohol (85%) 3 gal. 5 pt.
Sugar 20 Ib.
Water to make 10 gal.
Average Grade
Spirit of apricot stones 7 pt.
Alcohol (85%) i gal. 5 pt.
Sugar 10 Ib.
Water to make 10 gal.
Proceed as above.
ONE HUNDRED AND SEVEN YEARS
Cent Sept Ans
Spirit of lemon \\ gal.
Rose water 6 gal.
Alcohol (90%) 21 gal.
Sugar 100 Ib.
Water to make 100 gal.
Color strongly red with orchil.
ORANGE FLOWER CREAM
(Crime de Fleurs d* Granger)
Very Good Grade
Spirits of orange flowers i gal.
Orange flower water \ gal.
Alcohol (85%) 2 gal. i qt.
Sugar 35 Ib.
Water to make 10 gal.
LIQUEUR FORMULAE 221
Good Grade
Orange flower water 7 pt.
Alcohol (85%) 2 gal. 6 pt.
Sugar 20 Ib.
Water to make 10 gal.
Double Strength
Orange flower water i gal.
Alcohol (85%) 5 gal.
Sugan 20 Ib.
Water to make 10 gal.
Highest Quality "Synthetic"
Essence of French neroli oil 2 dr.
Orange flower water i pt. 9 oz.
Alcohol (85%) 4 gal.
Sugar 45 Ib.
Water to make 10 gal.
Average Grade "Synthetic"
Essence of neroli of Paris i dr. 16 min.
Alcohol (85%) 2 gal. 3 qt.
Sugar 20 Ib.
Water to make 10 gal.
PERFECT LOVE
(Par/ ait Amour)
Very Good Grade
Spirit of lemon i qt. 7 oz.
* ' * ' oranges i qt. 7 oz.
" " coriander 3 pt.
" " anis i qt.
Alcohol (85%) 2 gal.
Sugar 35 Ib.
Water to make 10 gal.
Color this or the following with orchil.
Good Grade
Spirit of lemon i qt. 7 oz.
" ' * coriander 3 pt.
Alcohol (85%) 2 gal. i pt.
Sugar 20 Ib.
Water to make 10 gal.
222 LIQUEURS AND CORDIALS
Average Grade
Spirit of lemon I pt. 8 oz.
' c ' ' coriander i pt. 8 oz.
Alcohol (85%) 2 gal. i pt.
Sugar 10 Ib,
Water to make 10 gal.
Average Grade "Synthetic"
Essence of distilled lemons 4 dr. 30 min.
' ' ' ' cedar ' i dr. 30 min.
" " coriander 6 min.
Alcohol (85%) 2 gal. 5 pt.
Sugar 10 Ib.
Water to make 10 gal.
PINEAPPLE LIQUEUR
(Crime d* Ananas)
Finest Quality
Pineapple (fresh) 6 Ib. 7 oz.
Alcohol (85%) 4 gal.
Crush and infuse pineapple in alcohol for 8 days. Filter through silk
cloth. Add sugar dissolved in 2% gallons of water. Add 7 oz. infusion
of vanilla. Color yellow with caramel.
PUNCH LIQUEUR
Brandy (58%) 5 oz.
Tafia (55%) 2 qt.
Spirit of lemon, concentrated i \ oz.
Citric acid I oz.
Hyswen tea i f oz.
Burnt sugar (4 B) 15 Ib.
Water 4 gal.
QUINCE BRANDY Ratafia de Goings
Sweet juice of ripe quinces 5 pt.
Spirit of cloves 7 oz.
Alcohol (85%) 2j gal.
Sugar 10 Ib.
Water to make 10 gal.
Color yellow with caramel.
LIQUEUR FORMULAE 223
ROSE LIQUEUR
(Huile de Roses)
Good Grade
Rose water i gal. i qt.
Alcohol (85%) 5 gal
Sugar 20 Ib.
Water to make 10 gal.
Average Grade "Synthetic"
Essence of roses 1 1 oz.
Alcohol (85%) 2 gal. 3 qt.
Sugar 20 Ib.
Water to make 10 gal.
STRAWBERRY CORDIAL
(Ratafia de Frambroises)
Finest Quality
Infusion of strawberries 3 gal.
" cherries i gal.
Alcohol (85%) i gal.
Sugar 40 Ib.
Water to make 10 gal.
Average Grade
Infusion of strawberries i gal. 2 qt.
" black currant 2 qt.
Alcohol (85%) i gal. I qt.
Sugar 10 Ib.
Water to make 10 gal.
STRAWBERRY BRANDY
Average Grade Double Strength
Spirit of strawberries (80%) 16 gal.
Alcohol (90%) 8 gal. i qt.
Sugar 200 Ib.
Water to make 100 gal.
TRAPPISTINE
(See note under "Benedictine")
Grand absinthe 5? oz.
Angelica 5? oz.
Peppermint 1 1 oz.
224 LIQUEURS AND CORDIALS
Cardamom 5^ oz.
Melisse (balm) 4 oz.
Myrrh 2^ oz.
Calamus 2 J oz.
Cinnamon i oz.
Cloves ^ oz.
Mace i oz.
Alcohol (85%) 4 gal. 2 qt.
Sugar 30 Ib.
Water to make 10 gal.
Follow the general methods for Benedictine.
VESPETRO
Very Good Grade
Spirit of amber seeds i pt.
" " dill i qt.
' ' ' ' anis 2 qt.
* ' ' ' caraway 2 qt.
* ' " coriander 2 qt.
' ' ' ' daucus i qt.
" fennel. i qt. i pt.
Alcohol (85%) i gal. i qt.
Sugar 35 Ib.
Water to make 10 gal.
Good Grade
Spirit of amber seed 7 oz.
< c< dill 21 oz.
' ' " anis i qt. i pt.
* * caraway i qt.
4 ' ' ' coriander I qt.
" " daucus ii oz.
" " fennel i qt.
Alcohol (85%) i qt. i pt.
Sugar 20 Ib.
Water to make 10 gal.
Average Grade
Spirit of amber seed 14 oz.
" ' 4 dill 14 oz.
14 " anis 28 oz.
LIQUEUR FORMULAE 225
Spirit of caraway 14 oz.
* ' ' ' coriander 28 oz.
" "daucus 14 oz.
" fennel 14 oz.
Alcohol (85%) 4 gal. i pt.
Sugar 20 Ib.
Water to make 10 gal.
Best Grade tl Synthetic"
Essence of anis 4 dr.
* ' " caraway 3 dr.
* ' " sweet fennel i oz.
' * ' * coriander 30 min.
' ' * * distilled lemon 2 dr.
Alcohol (85%) 4 gal.
Sugar 45 Ib.
Water to make 10 gal.
Average Grade "Synthetic"
Essence of anis 3 dr.
* * * * black currants 2 dr.
' ' " sweet fennel 40 min.
" " coriander 50 min.
' ' " distilled lemon i dr.
Alcohol (85%) 2 gal. 3 qt.
Sugar 20 Ib.
Water to make 10 gal.
CREAM OF VANILLA
Very Good Grade
Infusion of vanilla 3 qt.
Alcohol (85%) 2 gal. 2 qt.
Sugar 35 Ib.
Water to make 10 gal.
Color with cochineal or orchil.
Good Grade
Infusion of vanilla 2 qt.
Alcohol (85%) 2 gal. i qt.
Sugar 20 Ib.
Water to make 10 gal.
226 LIQUEURS AND CORDIALS
Average Grade Double Strength
Infusion of vanilla i qt.
Alcohol (85%) 4 gal. 3 qt.
Sugar 20 Ib.
Water to make 10 gal.
Average Grade Single Strength
Infusion of vanilla i pt.
Tincture of storax calamite 4 oz.
Alcohol (85%) 2 gal. 2 qt.
Sugar 10 Ib.
Water to make 10 gal.
BITTERS
These are a special group of liqueurs used for their tonic
properties and in small portions to flavor other beverages. In
general, their manufacture is simple and quality depends on the
proper selection of materials and care rather than intricate proc-
essing. A few formulae are cited below from the vast number
available. These are selected to be sufficiently illustrative. The
remainder, the matching of any preparation now on the market
is rather a matter for the master of the art than choice from a
receipt book.
Angostura Bitters
Angostura bark 31 Ib.
Red sandalwood 3 Ib.
Liquorice (wood) i Ib.
Chinese cinnamon f Ib.
Ginger root 10 oz.
Galanga root 10 oz.
Cardamom 10 oz.
Cloves 12 oz.
Orange peel 6 oz.
Mace , 3 oz.
Cut the materials up finely and macerate them for 8 days in 6 gallons
of alcohol (50%). Stir frequently. Add 40 gallons of alcohol (95%)
and 8 gallons of sugar syrup. Add water to make up to 100 gallons total
volume. Color reddish brown with caramel and tincture of cochineal.
LIQUEUR FORMULAE 227
Distilled Bitters
Orange peel 12 lb.
Dutch curacao bark 12 lb.
Gentian (chopped) 6 oz.
Cinchona bark 2 lb.
Calamus i lb. 4 oz.
Cardamom | oz.
Lemon peel 2^ lb.
Columba i J oz.
Tangerine peel 6 oz.
Alcohol (96%) 68 gal.
Water 100 gal.
Macerate for 48 hours. Distill to recover 75 gallons at So%.
Add:
Distillate 75 gal.
Caramel 5 ' '
Sugar syrup 10 * '
Water no "
200 gal.
Fine and filter.
Unicum Bitters
Sugar 80 lb.
Honey 64 lb.
Absinthe 5 oz.
Calamus root 2 oz.
Cinnamon bark I \ oz.
Ginger 2 oz.
Orange peel i \ oz.
Lemon peel i oz.
Centaury 2^ oz.
Gentian 2 oz.
Cinchona bark (red) i .oz.
Angelica root i oz.
Lemon balm i\ oz.
Spearmint i oz.
Rhubarb i oz.
Angostura bark 2& oz.
228 LIQUEURS AND CORDIALS
Macerate 3-7 days in 100 gallons 42% alcohol. Draw off, fine, and
filter.
VERMOUTH
(Sweet or Italian Type)
Absinthe i Ib.
Gentian i\ oz.
Angelica root 8 oz.
Blessed thistle i Ib.
Calamus root i Ib.
Starwort i Ib.
Centaury i Ib.
Forget-me-not i Ib.
Cinnamon 12 oz.
Nutmeg 2 oz.
Fresh cut oranges No. 24
Sweet white wine 93! gal.
Alcohol (85%) 5! gal.
Macerate 5 days. Draw off and fine. Let stand 8 days and fine again.
The product is then ready to bottle. Isinglass is preferred for fining.
Vermouth Dry or French Type
Coriander 4 Ib.
Bitter orange peel 2 Ib.
Orris root (powder) 2 Ib.
Cinchona bark (red) i Ib. 4 oz.
Calamus i Ib. 4 oz.
Absinthe i Ib.
Blessed thistle i Ib.
Star wort i Ib.
Centaury i Ib.
Germander i Ib.
Cinnamon 14 oz.
Cloves 7 oz.
Quassia 3i oz.
Dry white wine 100 gal.
Grind or crush the herbs, etc. Macerate 5-6 days. Draw off and
fine. Let stand 15 days and add 2 gallons of bitter almond shell extract
(see below) and three gallons grape brandy. The bitter almond shell
extract is made by macerating i part bitter almond shells in 2 parts of
85% alcohol for 2 months.
LIQUEUR FORMULAE 229
Vermouth Madeira Type
Absinthe i Ib.
Angelica root 8 oz.
Blessed thistle i Ib.
Lung moss i Ib.
Veronica i Ib.
Rosemary i Ib.
Rhubarb 4 oz.
Cinchona bark (red) i Ib. 12 oz.
Powdered orris root 2 Ib.
Curacao extract (see below) \ gal.
Madeira wine 91 gal.
Grape sugar 3 \ gal.
Old brandy 5? gal.
Macerate 3 days. Draw off and fine. Age 8 days and fine again.
The curagao extract is prepared by macerating i part Curasao peels in
2 parts of 85% alcohol for 8-10 days.
CHAPTER XIII
THE ANALYSIS OF ALCOHOLIC BEVERAGES
INTERPRETATION
General Statement. Materials in general and alcoholic
beverages in particular may be subjected to chemical analysis for
any of a great variety of reasons. These include among others
( i ) analysis by a manufacturer to determine uniformity of each
batch of product with preceding batches; (2) analysis to determine
the existence of adulteration in the product; (3) analysis to deter-
mine compliance with standards of quality such as the Federal
Pure Food Standards; (4) analysis to determine the identity of
the material (i.e., compliance with definitions) ; (5) and analysis
for the purpose of duplication of the material. Consideration
must always be given to the purpose of the analysis before actual
selection of the determinations to be made and the methods of
making them. Obviously, a manufacturer can check his product
from day to day by one or a few simple tests. On the other hand,
analyses made to determine the identity or to duplicate a product
must necessarily be as complete and as exact as the analytical art
will permit. With this possibility in view, the methods of analysis
cited in Chapter XIV have been reprinted, without exception,
from the Official and Tentative Methods of Analysis of the
Association of Official Agricultural Chemists, 3rd ed. 1930.
Grateful acknowledgment is here made to the Association for per-
mission to copy. These methods not only have official standing in
the courts and with governmental administrative bodies, but they
have been written after careful collaborative study so that they
are both exact and complete in detail.
Despite the accuracy and reproductibility of the results obtain-
able by the methods cited, the analytical chemist must confess that
230
GENERAL STATEMENT 231
his satisfaction of purposes 4 and 5 listed above, is difficult and
often impossible of completion. This difficulty arises partly out
of the inherent variability of many factors which enter into the
composition of alcoholic beverages. Among these are noted
especially the raw materials and the bio-chemical reactions of
fermentation. Part of the difficulty is also due to the fact that
the distinguishing characteristics of alcoholic beverages, flavor,
FIG. 49. Modern distillery laboratory. (Courtesy American Wine and Liquor
Journal.)
smoothness, aroma, etc., are intangible by the analyst and can only
be known by sensing them.
However, notwithstanding the difficulties stated, the analyst
has compiled data regarding the average composition of wines
and distilled beverages. Comparison of the results obtained by
the analysis of any given sample with the data so compiled will,
therefore, indicate the approach of the sample to the norm for
the kind of material it represents and may on occasion so empha-
size the abnormality of the material as to establish its non-agree-
ment with the definition.
232 ANALYSIS OF ALCOHOLIC BEVERAGES
Definitions. There can be no discussion of the meaning of
analysis of alcoholic beverages without prior agreement on the
meaning of the names applied to the beverages, i.e., definitions of
the beverages. Since the definitions and standards used by the
Food and Drug Administration of the U. S. Department of Agri-
culture and the labeling requirements of the Federal Alcohol Con-
trol Board have the force of law in this country, as well as the
merit of presenting definitions in as accurate language as pos-
sible, they have been adopted by the authors and are presented
here.
Definition of Whiskey. The Department of Agriculture de-
fines only medicinal whiskey and requires that it shall conform to
the definition contained in the U. S. Pharmacopoeia. This defi-
nition reads as follows : "Whiskey is an alcoholic liquid obtained
by the distillation of the fermented mash of wholly or partly
malted cereal grains, and containing not less than 47 per cent
and not more than 53 per cent by volume of C 2 H 5 OH at 15.56^.
It must have been stored in charred wood containers for a period
of not less than four years.
The pharmacopoeia also sets up certain standards of identity
and purity. These are:
Acidity (Calculated as acetic) 36-120 parts per 100,000
Esters (Calculated as ethyl acetate) 30-123 parts per 100,000
Solids (Extract) not over 500 parts per 100,000
Color To pass Marsh test for caramel.
Freedom from denaturants such as wood alcohol, diethylphthalate, for-
maldehyde, etc.
The Federal Alcohol Control Administration in a regulation
(Series 4) dated June 13, 1934 defines a number of classes and
types of whiskey which include :
Types:
Neutral whiskey, Straight whiskey, Straight rye whiskey, Straight
bourbon whiskey, Blended whiskey, Blended rye whiskey, Blended
bourbon whiskey, a blend of straight rye whiskeys, a blend 'of
straight bourbon whiskeys, Spirit whiskey, Scotch whiskey, Irish
whiskey, Blended Scotch whiskey, Blended Irish whiskey, Special
types of whiskey.
DEFINITION OF WHISKEY 233
The separate definitions of these are:
(a) Neutral whiskey is any alcoholic distillate from a fer-
mented mash of grain, distilled at more than 160 proof, and less
than 190 proof.
(b) Straight whiskey is any alcoholic distillate produced from
a fermented mash of grain, distilled at not exceeding 160 proof
and withdrawn from the cistern room of the distillery between
no proof and 80 proof, and produced by the same distillery
from the same type of materials, and as part of the same season's
distillation, whether or not such proof is reduced prior to bot-
tling.
(c) Straight rye whiskey and Straight bourbon whiskey are
straight whiskey distilled from a fermented mash of grain in which
rye or corn, respectively, are the principal materials.
(d) Blended whiskey is a mixture of straight whiskeys, or
of straight whiskey or whiskeys and neutral whiskey, or of
straight whiskey or whiskeys and neutral spirits distilled from
grain, which contains at least 20% of 100 proof straight whiskey
by volume.
(e) Blended rye whiskey, and blended bourbon whiskey are
blended whiskeys in which the whiskey or whiskeys are all rye or
all bourbon, respectively.
(f) A blend of straight whiskeys, A blend of straight rye
whiskeys, and A blend of straight bourbon whiskeys are mixtures
composed only of straight whiskeys, straight rye whiskeys, or
straight bourbon whiskeys, respectively.
(g) Spirit whiskey is a mixture of straight whiskey or whis-
keys and neutral whiskey, or of straight whiskey or whiskeys and
neutral spirits distilled from grain, which contains at least 5%
and less than 20% of 100 proof straight whiskey or straight
whiskeys by volume.
(h) Scotch whiskey is a distinctive product of Scotland (i)
composed of not less than per cent by volume of straight
whiskey or whiskeys distilled therein from a fermented mash of
barley malt, and of neutral whiskey distilled therein, and (2)
manufactured and blended in compliance with the laws and regula-
234 ANALYSIS OF ALCOHOLIC BEVERAGES
tions of the United Kingdom, and (3) containing no whiskey
less than three years old.
(i) Irish whiskey is a distinctive product of Ireland (i)
composed of spirits distilled at approximately 171 proof from
a fermented mash of malted barley and unmalted barley and other
grains, with or without the addition of other spirits similarly dis-
tilled in other seasons by the same distillery, and with or without
the addition of not more than per cent by volume of neutral
whiskey distilled at a higher proof, and (2) manufactured (in-
cluding blending if practiced) in accordance with the laws and
regulations of that division of Ireland in which manufactured, and
(3) containing no whiskey less than three years old.
(j) Blended Scotch whiskey or blended Irish whiskey is
Scotch whiskey or Irish whiskey that is in fact a mixture of
whiskeys.
(k) Special types of whiskey (i) Any person producing
any distilled spirits which, as a result of treatment by a chemical
or mechanical process, possess the taste, aroma, characteristics
and chemical composition of any whiskey for which standards of
identity are herein prescribed, may petition the Administration for
permission to designate such distilled spirits as whiskey of some
new type, and the Administration may take such action on such
petition as it deems fair and reasonable. (2) Any whiskey of
any class or type prescribed in paragraphs (b) to (g) above,
inclusive, produced in a foreign country, shall be designated by
the name of the country in which produced, together with the
applicable designation prescribed in such paragraphs.
OTHER DISTILLED LIQUORS
The F. A. C. A. classes and definitions are :
Gins
(a) "Distilled gin" and "compound gin" without appropriate
qualifying words, are distilled gin and compound gin, respectively,
in which the predominant flavor is derived from juniper berries.
(b) Distilled gin is the product obtained by distilling juniper
berries or other similar flavoring materials with neutral spirits.
OTHER DISTILLED LIQUORS 235
(c) Compound gin is the product obtained by mixing dis-
tilled gin or gin essence or similar gin flavoring material with
neutral spirits.
(d) "London Dry," "Hollands," "Plymouth," "Geneva,"
"Old Tom," "Buchu," and "Sloe" gin are the types of gin known
to the trade under such generic designations, and "distilled gin"
or "compound gin," whichever is appropriate, shall accompany
such designations.
BRANDIES
(a) Brandy is the alcoholic distillate obtained solely from
the fermented juice of fruit, distilled under such conditions that
the characteristic bouquet or volatile flavoring and aromatic
principles are retained in the distillate.
(b) "Brandy" without appropriate qualifying words, and
"Grape Brandy" are the distillates obtained from grape wine or
wines under the conditions set forth in (a).
(c) Apple Brandy, Peach Brandy, or other fruit brandies
are distillates obtained from the fermented juice of the respec-
tive fruits under the conditions set forth in (a).
(d) Cognac and Cognac Brandy is grape brandy distilled in
the Cognac region of France, which is entitled to be designated
as "cognac" by the laws and regulations of the French govern-
ment.
RUM
(a) Rum is any alcoholic distillate obtained solely from the
fermented juice of sugar cane, sugar cane molasses, or other
sugar cane by-products, in such a manner that the distillate pos-
sesses the taste, aroma, characteristic and chemical composition
generally attributed to rum, and known to the trade as such.
WINES
The Department of Agriculture definitions of wine have been
readopted since the repeal of prohibition from those promulgated
on June 12, 1914. They read as follows:
i. Wine is the product made by the normal alcoholic fer-
mentation of the juice of sound ripe grapes, and the usual cellar
236 ANALYSIS OF ALCOHOLIC BEVERAGES
treatment, and contains not less than 7 per cent or more than 16
per cent of alcohol, by volume, and, in 100 cubic centimeters
(2OC.) not more than o.i gram of sodium chloride nor more
than 0.2 gram of potassium sulphate; and for red wine not more
than 0.14 gram, and for white wine not more than 0.12 gram of
volatile acids produced by fermentation and calculated as acetic
acid. Red wine is wine containing the red coloring matter of the
skins of grapes. White wine is wine made from white grapes or
the expressed fresh juice of other grapes.
2. Dry wine is wine which the fermentation of the sugars
is practically complete, and which contains, in 100 cubic centi-
meters (2OC), less than i gram of sugars and for dry red wine
not less than 0.16 gram of grape ash and not less than 1.6 grams
of sugar-free grape solids, and for dry white wine not less than
0.13 gram of grape ash and not less than 1.4 grams of sugar-
free grape solids.
3. Fortified dry wine is dry wine to which brandy has been
added but which conforms in all other particulars to the standard
of dry wine.
4. Sweet wine is wine which the alcoholic fermentation has
been arrested and which contains, in 100 cubic centimeters
(2OC.), not less than i gram of sugars, and for sweet red wine
not less than 0.16 gram of grape ash, and for sweet white wine
not less than 0.13 gram of grape ash.
5. Fortified sweet wine is sweet wine to which wine spirits
have been added. By act of Congress, "sweet wine" used for
making fortified sweet wine and u wine spirits" used for such forti-
fication are defined as follows (sec. 43, act of Oct. i, 1890, 26
Stat. 621 ; as amended by Sec. 68, act of Aug. 27, 1894, 28 Stat.
568; as amended by sec. i, act of June 7, 1906, 34 Stat. 215; as
amended by sec. 2, act of Oct. 22, 1914, 38 Stat. 747; as amended
by sec. 402 (c), act of Sept. 8, 1916, 39 Stat 785 ; and as further
amended by sec. 617 act of Feb. 25, 1919, 40 Stat. mi):
That the wine spirits mentioned in section 42 is the product re-
sulting from the distillation of fermented grape juice, to which
water may have been added prior to, during or after fermenta-
tion, for the sole purpose of facilitating the fermentation and eco-
OTHER DISTILLED LIQUORS 237
nomical distillation thereof, and shall be held to include the
product from grapes or their residues commonly known as grape
brandy, and shall include commercial grape brandy which may
have been colored with burnt sugar or caramel; and the pure
sweet wine which may be fortified with wine spirits under the
provisions of this act is fermented or partially fermented grape
juice only, with the usual cellar treatment, and shall contain no
other substance whatever introduced before, at the time of, or
after fermentation, except as herein expressly provided: Pro-
vided, That the addition of pure boiled or condensed grape must
or pure crystallized cane or beet sugar, or pure dextrose sugar
containing, respectively, not less than 95 per centum or actual
sugar, calculated on a dry basis, or water, or any or all of them,
to the pure grape juice before fermentation, or to the fermented
product of such grape juice, or to both, prior to the fortification
herein provided for, either for the purpose of perfecting sweet
wines according to commercial standards or for mechanical pur-
poses, shall not be excluded by the definition of pure sweet wine
aforesaid: Provided, however, That the cane or beet sugar, or
pure dextrose sugar added for sweetening purposes shall not be
in excess of 1 1 per centum of the weight of the wine to be forti-
fied : And provided furthur, That the addition of water herein au-
thorized shall be under such regulations as the Commissioner of
Internal Revenue, with the approval of the Secretary of the
Treasury, may from time to time prescribe : Provided, however,
That records kept in accordance with such regulations as to the
percentage of saccharine, acid, alcoholic, and added water con-
tent of the wine offered for fortification shall be open to inspec-
tion by any official of the Department of Agriculture thereto duly
authorized by the Secretary of Agriculture; but in no case shall
such wines to which water has been added be eligible for forti-
fication under the provisions of this act, where the same, after
fermentation and before fortification, have an alcoholic strength
of less than 5 per centum of their volume.
6. Sparkling wine is wine in which the afterpart of .the
fermentation is completed in the bottle, the sediment being dis-
gorged, and its place supplied by wine or sugar liquor and/or
238 ANALYSIS OF ALCOHOLIC BEVERAGES
dextrose liquor, and which contains, in 100 cubic centimeters
(2OC), not less than 0.12 gram of grape ash.
7. Modified wine, ameliorated wine, corrected wine, is the
product made by the alcoholic fermentation, with the usual cellar
treatment, of a mixture of the juice of sound, ripe grapes with
sugar and/or dextrose, or a sirup containing not less than 65 per
cent of these sugars, and in quantity not more than enough to
raise the alcoholic strength after fermentation to n per cent by
volume.
FOOD INSPECTION DECISION 156
As a result of investigations carried on by this Department
and of the evidence submitted at a public hearing given on Novem-
ber 5, 1913, the Department of Agriculture has concluded that
gross deceptions have been practiced under Food Inspection De-
cision 1 20. The department has also concluded that the defini-
tion of wine in Food Inspection Decision 109 should be modified
so as to permit correction of the natural defects in grape musts
and wines due to climatic or seasonal conditions.
Food Inspection Decisions 109 and 120 are, therefore, hereby
abrogated and, as guide for the officials of this Department in
enforcing the Food and Drugs Act, wine is defined to be the
product of the normal alcoholic fermentation of the juice of fresh,
sound, ripe grapes, with the usual cellar treatment.
To correct the natural defects above mentioned the follow-
ing additions to musts or wines arc permitted:
In the case of excessive acidity, neutralizing agents which do
not render wine injurious to health, such as neutral potassium
tartrate or calcium carbonate;
In the case of deficient acidity, tartaric acid;
In the case of deficiency in saccharine matter, condensed grape
must or a pure dry sugar.
The foregoing definition does not apply to sweet wines made
in accordance with the Sweet Wine Fortification Act of June 7,
1906 (34Stat. 215).
A product made from pomace, by the addition of water, with
or without sugar or any other material whatsoever, is not entitled
CORDIALS AND LIQUEURS 239
to be called wine. It is not permissible to designate such a product
as "pomace wine," nor otherwise than as "imitation wine."
CORDIALS AND LIQUEURS
Cordials are defined by the Department of Agriculture as
follows :
Food Inspection Decision No. 125 July 7, 1910
The Labeling of Cordials
"The term 'cordial' is usually applied to a product, the alcohol
content of which is some type of a distilled spirit, commonly neu-
tral spirits of brandy. To this is added sugar and some type
of flavor. The flavor is sometimes derived directly by the addi-
tion of essential oils, again by use of synthetic flavors, and also
by the treatment of some vegetable product with the alcoholic
spirit to extract the flavoring ingredients. It is likewise the gen-
eral custom to color cordials. When a cordial is colored in such
a way as to simulate the color of the fruit, flavor, plant, etc.,
the name of which it bears, the legend 'Artificially Colored' in
appropriate size type shall appear immediately beneath the name
of the cordial, as is required by Regulation 17. Where the
color used is not one which simulates the color of a natural
product, the name of which is borne by the liqueur, then the
legend as to the presence of artificial color need not be used.
For example, creme de menthe which is artificially colored green
should be labeled 'Artificially Colored.' On the contrary, char-
treuse, whether green or yellow, need bear no such legend for
color.
"When the flavoring material is not derived in whole directly
from a flower, fruit, plant, etc., the name of any such flower,
fruit, plant, etc., should not be given to any cordial or liqueur
unless the name is preceded by the word 'Imitation.' "
The F. A. C. A. definition of cordials and liqueurs is:
(a) Cordials and Liqueurs are the products obtained by dis-
tilling fruits, flowers, plants, leaves, roots, or other flavoring ma-
terials, except gin flavoring materials, with brandy or neutral
2 4 o ANALYSIS OF ALCOHOLIC BEVERAGES
spirits, and to which sugar has been added; or the products ob-
tained by mixing fruit juices, essential oils and flavoring materials,
other than gin flavoring materials, with brandy or with neutral
spirits and to which sugar has been added.
Imitations. The attitude of the Department of Agriculture
has always been that any product which simulated those for which
it has definitions and standards, but does not fully comply there-
with, is an imitation. The F. A. C. A. has actually set forth
definitions of imitations.
(a) Imitation whiskey is any distilled spirits containing rye or
bourbon essential oils or essences, or any distilled spirits colored
or flavored in imitation of whiskey; and the designation
"Whiskey" shall not be used unless immediately preceded by
"Imitation."
(b) Imitation cordials and liqueurs. When the flavoring
material of a cordial or liqueur is not derived in whole directly
from a fruit, flower, plant, leaf, root or other flavoring material,
the name of any such fruit, flower, plant, leaf, root or other
flavoring material shall not be given to the cordial or liqueur
unless the name is immediately preceded by the word "Imitation."
(c) Imitations, other than (a) and (b) above, are distilled
spirits colored or flavored in imitation of any class or type of dis-
tilled spirits defined in these Regulations, and the name of such
class or type of distillated spirits shall not be used unless imme-
diately preceded by the word "Imitation."
Finally, the F. A. C. A. has set forth certain regulations
of interest, regarding geographical names and additions of color-
ing, etc.
Section i. (a) Geographical and distinctive names. The
name for distilled spirits which have a geographical name, or
which are distinctive products of a particular place or country
shall not be given to the product of any other place or country,
unless such name is immediately followed by the word "type,"
and unless such product in fact conforms to such distilled spirits
except as to age.
(b) This section shall not apply to designations which by
reason of usage and common knowledge have lost their geo-
ANALYSES OF WHISKEY 241
graphical significance to such an extent that they have become
generic, provided the approval of the Administration is obtained
prior to using such designation.
Section 2. Coloring and Flavoring Materials. The addition
of harmless coloring or flavoring materials, such as burnt sugar
and blending materials, in a total amount not in excess of 2j^%
of the distilled spirits by volume, shall not alter the classifica-
tion of any distilled spirits as defined in these Regulations, pro-
vided such coloring or flavoring materials are not used to imitate
any class or type of distilled spirits for which standards of identity
are established herein. This section shall not affect cordials or
liqueurs.
It will have been noted by the reader that the definitions just
cited are in general based on the principle of stating that a
product bearing a given name must be made from the materials
commonly used in the manufacture of that product, by the com-
monly understood processes of manufacture. // is only as a corol-
lary that one may deduce that the composition of the product
must conform to the general average of the type within reasonable
limits. In order that the reader may judge for himself the fact
of this compliance, a selection of the published analytical data re-
garding liquors is presented here. The tabulated analyses of
whiskey were made at the end of the first decade of this century.
The "pure food" movement both here and abroad was then at
its crest, and the question, "What is whiskey" was considered at
length by legal bodies. The analyses presented were generally
used as evidence in public hearings.
ANALYSES OF WHISKEY
British. Shidrowitz (Royal Commission of Whiskey and
other Potable Spirits. Minutes of Evidence, Vol. i, pages 409,
410, 1909) reports analyses of Scotch and Irish pot and patent
still whiskeys and of American Bourbons and Ryes as follows :
242 ANALYSIS OF ALCOHOLIC BEVERAGES
B "8
f*
o
ii
^ "i
< CO
-5
W
S
as,
1
^O
o
n
CO JU
s2 -
1 S
"2
2
(2
Aldehydes
*
11!
O oo
f- OO
2
-5
w
**
o>
O rt "u
'Ctf r^
^s
CO OO
C
2 S
;
w g.
Alcohol
per cent
by volume
l
oT
c
3
i
8 JS
J '~
^1
5^> ^ ?^
1 1 1
Q Q
ANALYSES OF WHISKEY
243
II
II
.
fe
5 ^
5 o
co e
co
1 1
ift
X
w
-J
S
1
O d M
6 o
1
HI
* as ,
1
?-?*
C '3 ^
O rt "53
~O rt
O co -^
"rt T3
'
rf Tf -^- 00
o C
2 o
t -
w S.
o" o ts
666
-J S J3
- fe ^
^J- v,^ f^ OO
O O ON CT\
\O ^ l -o -o
1 ,
J>- "Tj O
^QO
^ CO j ^g
^ 2 PL, CO
^ C 2
1 !!
3SSS
^
S
53
1
^
"2
2
1
88 8^
r? E? t? 2
H H H
1
>
JZ
<U
T3
<
CO MM
Jl^
W) O '.
s-^<
oo O co c< so O
CO *^* -^f -O rf *-^
2
s
W
vr> H tj- CTs ^n CO
CS rt- C t~< <H CO
OJ
C '"5 T3
O <rt 'Q
Z| -
Tf HH CO
CO
"3 T3
o *C
^2
r^ w o ro cr
i C< *-i
t; s
c V
"
o 8
>< h
w g.
o>
* J C
5 g 1
. "1
<-^
vo r-- c * <$
r>v oo r>. o\ co vo
6 ON 6 HH" ON i-i
[\ \o r>- r-- vo r^
: ; 2 ; s ;
s 3s" s
2- X 2J
XL, ^ ^ /^
^ OQ Cj
1: = 1: I
'5 .S .?
3 Q Q
"S
o
I
I
244 ANALYSIS OF ALCOHOLIC BEVERAGES
i
Q
I
I
c!
73
vn co M ^ v*so <H ON * osvO t- c^
i
1
*^co^t-^^t-c< COCOCOCOCOC<M
Q
8
1
ng
s - aM a ea5a
1
*li
*-o vr% co ^ V O r** r*^ ON !"" OO |^- O OO O
I
S -8
w
^oooor^-r^ON ONOO^-HHVOJ-IONON
aH*
OO OO^^O OOONON-ii-tOO N O
TC* '^fCO^t'' T t'COCi>-<>-
II 1
S (14 S
B.-S
O <->
S VO d * H CO
*"" S NV co oo" v~ 2 ci S TJ- \2 co oo r- v?
H *
5 -----
C/5
o J2 b
il
CO
W
O Oc<- Ui i-<vri-i>-(-icSvOC<
= 1 S
.a l
O OOO gj OOOOOOOO
ft) OJ
3 S |
^ -3
COOi-r--.CST|- < OOO-C<OOVOr^ON
l- in ^
^^ 3 ^
^r^rj-dcovd g oXr^vdo\v>vo"4;*o
S i "-
< *J3
J5
1* 1 g
III
i^iili !i i; i ! ii
A CO CO
7^ ^s. *"
];*'
^ . ^ co' *>
e c fc b 3 .-..
'3 '3 8 1 : J J ti e
-^ ^^ f* ^- W . U 1) W l-
^ ^ ^S " p S p S
S2 s2t2oj iiS^
rt ctirtK '. ' ^* S 5 5
>' ^ > > >L '^J^^^^'VV
^ 4> ^ eg 1 1 1 1 1
1; ~\ ~r\. |: ^ Gc 5^
Note re American Whiskie
Both the Bourbon samples anc
Note. Except where oth(
ANALYSES OF WHISKEY
X
II
.3
-a
o
Si -g
J 1 S
PQ
4> O O
S c.S
^ ^ s
c "3 a
O^o
e "* u
1
H fi
s e
% J2 <->
^ <* O O oo so
-* rf-so d O -<*
^0
Jb r-; ^
so oo oo d ^^ so
O^v co O I*"" t^- O
&
sl^
SO t~- f v/ ~> OO ^ p
d -^- r- oo I-* u^>
d co d -o
v
&
$ * q
.
_^
u 1 ocT
8
^
<t- d O ^O O oo
*^*^ d oo d ^t-
r>
^
d vo o <<*<* O
.S - c^vo
a.
fa
DH 8 -
Wo 1 - 1
s
CTl
X 2 IT
W H J
r
4 S
oo O O so d Tf-
oo d O ^ * d
"o
*~* P
r-- so o r~-* r- ^t-
t^* so o o> so r-
^3
< US
' HH OO d Tf"
CO >*H rf-
X
CO
so oo oo O ^ O
O oo oo so O O
g
O d oo r-~ r^ O
*-*~ d i^ co 0^1 O^s
"o
^* * O O co
oft
w
-, d
HH d
,0
rt
<u
O O O oo O so
s'J-'S
^ O *
d d O - co co
O O so ^- *
I
_
r^ d so so ^f oo
^- d so so oo *$-
^
o * C
*"* ^ 1-1 co
HH co co O so
d)
cx
CO
d so O oo d O
d ^- O oo so O
i
CO
vo co O r^ oo d
vo vo O ^ >- O
<
>-< l-i CO
co d so
c
O
O O O d O ^
O O oo so so sO
(X
in
d r~-* d co so so
so O d oo so ^
**
(3
co "<$ c<
- z ><*
g e Eg
u 3 <u a
OJQ c CD c e
etf S "* .5 C!
S g S g
<u D S o a
SP. e P e !
^
fe rt '^ ** rt "^
< ^ < ^
g s ; % :
< s s < s s
H"
03
CO
5 !s
i
-S Is
S
s en
s
& 1 ^
(A CO
00 W->
V
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1
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1
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1 i
246 ANALYSIS OF ALCOHOLIC BEVERAGES
w
&
w
2
X
w
I
4 R
<
Alcoho
<
I
8
2
O
Aldehydes
"3
W
acid
Vola
< i *- G
fi
*
O
3
rt
fc
H vo vovo VO O O M
vo O O M
M r^-<oo
"NO
vo
-g
"
S
ON
si,
^1
-
f
co O
.
S
"H
6
vo
<u ^
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I e
4
B
.S
"E
4J co
Ui
^ 1
ANALYSES OF WHISKEY
247
The maximum and minimum limits obtained by Schidrowitz
on 58 samples of Scotch whiskey regardless of age are shown in
Table XL (Royal Comrn. on Whiskey, etc., Minutes of Evi-
dence, Vol. i, p. 416, 1909.)
TABLE XI. MAXIMUM AND MINIMUM RESULTS OF ANALYSES ON FIFTY-EIGHT SAMPLES
OF SCOTCH WHISKEY. ANALYSES BY SCHIDROWITZ.
Non
Higher
Higher
Whiskey
Total
acid
vola-
tile
or\A
Ether
alcohols,
color-
imetric
alcohols,
Allen-
Marquardt
Alde-
hydes
Fur-
fural
method
method
Highland Malts. . .
10-83
-35
33-^5
328-864
112-235
4-66
1.6-6.3
Lowland Malts
6-60
0-16
27-87
189-897
82-228
8-54
0-5.2
Campbel towns
I 2-1 CO
0-28
53-Ho
357-93
160-259
11-85
2.4-8.0
Islays
ic-i6
o n
40-86
62074.0
I C C-2OO
17-40
1.8-C.2
Grains
7-60
0-26
2O-CC
19-400
^-80
tr.-i7
O-O.Q
Note: results are calculated to a basis of parts per 100,000 of absolute alcohol.
Another series of analyses made by Tatlock on 75 samples
of Scotch, Irish and American whiskies are shown in Table 12
(Tatlock, Royal Comm. on Whiskey, etc., Minutes of Evidence,
Vol. i, p. 431, 1909-)
248 ANALYSIS OF ALCOHOLIC BEVERAGES
" O
I
M
w 7
<d
w *>
1!
la
* S
< b
1i
s^ ?
l<
^S<o
Sis P
IJ OT
Jjeg
Kd!
s <2
(2
J
r p*
voso so *^> M SO
^25 3^$ ?& v?SJ? IgK 28g
1
a
00
J
"ft
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3
o
jU
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a
M
V
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a
00
a
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d cooo t-i oo o
85?* -* - ^a H & =^
4
c o
'23
"
V^ V> if "o* Q O *0
H M d >" co M c/i
American,
4 samples
d s> os if *-o Os M ^ co *o ** co so *^ Q d so Os Q Q Q oo M vo
^o O Os co *o Os M d ^f oo O **" oo os O Os r^-oo OOO *o d Os
?:::? f^g^
d <^ os d r^so co M co d oo \o Q Q O vrso -^
M ifcococo^d vo co ^
J
-cT o*
si
HM g
d
d if co - Os O
4"f
d ^>oo M co r^ O r^-oo soooo OOO M i- M
if oo M os if d
TT co ^- so ^o^O
<f d d HI so d if ddd oooooo
III
Cl 4J Cfl
U d
d d d O oo if
S^^ 8 fcffS, ^Ss 888 ^^S
w> HI co so Os co
00x0 ^ ^ ?J^
sOi-ico codd cococo ^n r--so O O ^ Osoo oo
rf
ji
^
O co v> r^ d ^>
HI HI so if d O Os *^~> d osift^ QQQ M S? ^
^ HI oo r^-oo ^f ddO OsOsco OOO do *^>
oo oo M M o ^
at;? R ? -- IH ff| 2^
i C
O d os so o\ o
vO O vr> Os O d vr> vr Os M d CO OOO vriOO OO
oor-co *or-if oosoco 00*^0 OOO w% HSO
w^ if so O co O
oo co^O if O "f
Osifr^- co if O vr d if if oo d O Os O oo so
co^cod M> _oo^ Os\O oo d Os
Highlands,
31 samples
so MSO O -" *-*
MQO if v o v O
*
so vo oo so -< oo if oo os v\Tj-H* QQQ ^ 'f oo
Or^^ Od^f co*^ 1 "" coOsif OOO sO'rO
if vr co Q ^ "t
vo if oo as r- if
OSHIM t/^coOs f^-Hiif dooif QO *^ ^O O * H
1-1 codd ifnid v^dif
co ' ' '
ill II! ill ill III 111,1112 lill
: ; : : : : : : : : : : : : : : : g : : : : : :
. : : a . . .Q ...
u v
: : : : : : : : :s : : :1 : : :i : : :
3 -H -T3
: : : : : : : : :| :::,-::: 8 : : :
: : . : j> ft : i> ^ : : R . : &
ia'BiiaBsS'e'B aS iafi|isS|iaSl |s!
II &1 11 5-11 I^ S If 5 |lSll|^j|S|..l|S
1:s s^'Sii ? 2 s:s s-s a:i s-s s: g a:s a" 3 s: g i g's: g
gss^sastS'-SsspJ&asiSlssfS^sssassiS-lssiS
2 -Ejs ^ ^: 2 "g, 3S
*tJ . O --s 3 O ; O^
ANALYSES OF WHISKEY 249
ANALYSES OF WHISKEY
American. There are available two extensive sets of analy-
ses of American Whiskies completed in the years 19091912.
The first set made by Crampton and Tolman (J. A. C. S. V.
XXX (1908), 98 et. seq.) was made in an investigation of the
effect of aging on whiskey. They drew samples each year for
4-8 years from the same barrels of whiskey stored in warehouses
and subjected these to extensive comparison. A summary of the
results follows.
It is of great importance in the interpretation of whiskey
analyses to note the conclusions obtained by Crampton and Tol-
man from their investigation.
"i. There are important relationships among the acids,
esters, color, and solids in a properly aged whiskey, which will
differentiate it from artificial mixtures and from young spirit.
2. All of the constituents are undergoing changes as the
aging process proceeds, and it is evident that the matured whis-
key is the result of these combined changes.
3. The amount of higher alcohols increases in the matured
whiskey only in proportion to the concentration.
4. Acids and esters reach an equilibrium, which is main-
tained after about three or four years.
5. The characteristic aroma of American whiskey is de-
rived almost entirely from the charred package in which it is
aged.
6. The rye whiskies show a higher content of solids, acids,
esters, etc., than do the Bourbon whiskies, but this is explained
by the fact that heated warehouses are almost universally used
for the maturing of rye whiskies, and unheated warehouses for
the maturing of Bourbon whiskies.
7. The improvement in flavor of whiskies in charred pack-
ages after the fourth year is due largely to concentration.
8. The oily appearance of a matured whiskey is due to ma-
terial extracted from the charred package, as this appearance is
almost lacking in whiskies aged in uncharred wood."
250 ANALYSIS OF ALCOHOLIC BEVERAGES
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ANALYSES OF WHISKEY
251
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252 ANALYSIS OF ALCOHOLIC BEVERAGES
"9. The 'body' of a whiskey, so-called, is due largely to the
solids extracted from the wood."
Adams J. Ind. & Eng. Ch. 3, 647 (1911) reports the results
of an " Investigation to detect substitution of spirits for aged
whiskey." His analytical results were similar to those of Cramp-
ton and Tolman (loc. aV.), but his conclusion merits repetition.
This is particularly the case because the question was passed on
by a Federal Court and his conclusions approved by the Court.
He states "In conclusion it should be stated that in work of this
kind, the acids, esters and color form the points which should be
used to determine the authenticity of the contents of a package of
whiskey. The content of solids, higher alcohols, aldehydes and
furfural will assist in arriving at a conclusion, but should not be
relied on solely as can be done in the case of the acids, esters,
and color."
Analyses of Typical Brandies. Girard and Cuniasse ("Man-
uel Pratique de L' Analyse des Alcools," 1899) state ^ at ^ e
sum of the secondary constituents, referred to as the "coefficient
of impurity," is seldom less than 300 in genuine brandy made from
wine. They give various analyses of brandies from which the
following have been chosen :
TABLE XV. ANALYSIS OF EAUX-DE-VIE DE VIN OF KNOWN ORIGIN.*
Cozes,
1874
Gemozac,
1*93
Gemozac,
1896
Champagne,
15-20 yrs.
Acidity
2O I .O
IOO 4.
2Q O
in. 8
Aldehydes.
4.6.
72.1
II C
7O. O
Furfural
0.4
0.8
1.2
1.6
Esters
QC.I
I1Q. I
JOI. 1
117.2
Higher alcohols
2C4.O
221.7
26o.O
24.4.. O
Total secondary constituents * .
Density at 1 5
596.5
O.QC7I
494-3
O . QO7 C
403.0
o 9022
524.6
Alcohol, by volume
TJ . O
64.. c
66 o
ro.o
Extract, per 100 cc
v^.. 3
I?' ^
O.2
* Expressed as parts per 100,000 of absolute Alcohol,
ANALYSES OF WHISKEY
253
TABLE XVI. ANALYSIS OF EAUX-DE-VIE OF KNOWN ORIGIN. *
(Analyzed in 1896)
Saintonge,
1880
Saintonge,
1896
Armagnac,
40 yrs.
Acidity
IOC. 7
17. <
14.6. 7
Aldehydes
27.Q
I'D
21. Q
11.4.
Furfural
2. 1
2 6
O.7
Esters
167 o
6l Q
I2C {
Higher alcohols
i CQ. 8
2 Co. 8
2OT. C
Total secondary constituents *
4.62.7
^6c.7
CO7.8
Density at 1 5
O.QI C7
0.804.7
Alcohol by volume
Co.o
68.2
40.8
Extract, per 100 cc
Nil
o. 18
* Expressed as parts per 100,000 of absolute alcohol.
These analyses tend to demonstrate the following changes
brought about by aging:
1 i ) Increase in acidity
(2) Increase in aldehydes
(3) Increase in esters
(4) Decrease in furfural
(5) Decrease in higher alcohols
(6) Decrease in total alcohol
Other analyses of unidentified brandies listed as commercial
cognacs and thought to be wine brandy cut with rectified alcohol
showed total secondary constituents ranging from 202 to 283.
These were compared with analyses of industrial alcohol (al-
cools d'industrie) showing total secondary constituents ranging
from 9 to 40.9.
Ordonneau (Compt. rend. 102, 217) subjected 100 litres of
25-year-old brandy to fractional distillation and reports the
following :
254 ANALYSIS OF ALCOHOLIC BEVERAGES
TABLE XVII. ANALYSIS OF 25-YEAR OLD BRANDY.
Grams per
Hectolitre
Aldehyde 3.0
Normal propyl alcohol 40.0
Normal butyl alcohol 218.6
Amyl alcohol 83. 8
Hexyl alcohol 0.6
Heptyl alcohol 1.5
Acetic ester 35.0
Propionic, butyric and caproic esters 3.0
Oenanthic ester (about) 4.0
Acetal and amines Tr.
W. Collingwood Williams (J. Soc. Chem. Ind., 1907, 26 y
499) gives results of analyses of 28 samples of Jamaica rum as
follows :
TABLE XVIII. ANALYSES or JAMAICA RUM.*
Min.
Max.
Average
Ordinary type. 21 samples
Alcohol, vol. per cent
68.6
82.1
70. I
Total solids, gms/ioo cc
O. I
1.16
0.4.7
Total acid as acetic
10
KC
78 c
Volatile acid
21
146
/o. ^
61
Esters
88
ioc8
166. c
Higher alcohols
4.6
I CO
08 c
i .0
* J^
II. C
yo. ^
A, f
Aldehydes
c.o
70.0
*r* J
ir.-7
Flavored rum. 7 samples
Alcohol* vol. per cent
66.1
80.6
77.1
Total solids, gms/ioo cc
Nil
0.61
0. 11
Total acid as acetic
At
14^
IO2. C
Volatile acid
'JO
IT7
of. e
Esters
W
1204
768.<
80
14.4.
IO7
2.7
12.
r.2
Aldehydes
1^. O
17- 5
20.7
* Results expressed as grams per 100 litres of alcohol (except the alcohol and solids).
J. B. Harrison (Official Gazette, Demerara, Oct. 19, 1904,
Extract, 2,093) Government Analyst, believes that a character-
ANALYSES OF WHISKEY
255
istic commercial Demerara rum would yield 70 to 80 parts of
esters per 100,000 of alcohol. He gives figures for various
Demerara rums as follows.
TABLE XIX. ANALYSES OF DEMERARA RUM.
AVERAGE
VALUES
Origin
Esters
Vol. acid
Distilleries in Demerara County
<A 7
26 c
" " Essequilo "
7Q. C
xu. $
11 O
" " Berbice "
17' J
78.7
jo- v
11 O
Continuous and Coffev stills
4.4.. Q
18.4.
Vat stills
60 Q
11. 1
wy.y
Bonis (Ann. Falsif. 1909, 12, 521) gives the following re-
sults of analyses of Martinique rum:
TABLE XX. ANALYSES OF MARTINIQUE RUM.
Vol.
acid
Esters
Aldehydes
Higher
alcohols
Furfural
20 1
443
92
68
8.8
High quality
201
J 74
9 1
93
59
32
385
425
5-3
II.
165
62
34
339
0.9
Average quality
'73
H5
83
118
20
23
244
167
o-5
6-3
197
95
16
97
3-8
Poor quality
158
90
15
143
O.I
53
5i
10
280
o-7
On fixed acids, the first sample showed 2.2 per cent and the
balance ranged from 0.37 to 0.95 per cent.
Girard and Cuniasse ( "Analyse des Alcools et des spiritueux" )
claim the average proportion of esters and other secondary prod*
ucts comprised in the non-alcohol coefficient found in ordinary
256 ANALYSIS OF ALCOHOLIC BEVERAGES
rums of commerce known to be genuine, are shown in the follow-
ing table, expressed as parts per 100,000 parts of absolute
alcohol :
TABLE XXI. AVERAGE PROPORTION OF ESTERS AND OTHER SECONDARY PRODUCTS AND
THE NON-ALCOHOL COEFFICIENT OF COMMERCIAL RUM.
Min.
Max.
Average
Acidity (as acetic acid)
IC8.4
400.0
2 CO. 8
Aldehydes (as acetaldehyde)
O. 1
C.4. c
24.4
Furfural
1.2
co.o
7. I
Esters (as acetic ester)
IOC. 7
447. I
220. C
Higher alcohols (isobutyl standard)
<2.O
7O8.6
140.4
Coefficient of secondary products
4.72.7
QIQ.O
6C2. C
Analyses of Gin. Since gin consists of a highly rectified
alcohol or spirit with flavor, little can be learned from its analysis.
However, Vasey ( u Analysis of Potable Spirits," p. 85) cites the
following results :
TABLE XXII.
Volatile acids o.o grams per 100 liters of absolute alcohol
Esters 37.3 " " " " "
Aldehydes 1.8 " " " " "
Furfural o.o " " " " " " "
Fusel oil 44.6 " " " " "
Analyses of Wine. There are reprinted here two extensive
tabulations of the analyses of European and American wines
respectively. The European Wine analyses (Table XXIII)
were compiled by Konig and are copied from Leach ("Food In-
spection and Analysis," 4th ed., 1920, p. 717). The American
Wine Analyses (Table XXIV) were compiled by Bigelow and
are copied from Leach (loc. cit., p. 718).
Bioletti ("Principles of Wine Making, 1 ' California Ag. Exp.
Sta., Bui. No. 213) summarizes the composition of wines as
follows :
The alcohol and acid in natural wines vary in an inverse
ratio, in such a way that the volume percentage of alcohol added
to the grams per liter of acid as sulfuric make a sum lying be-
ANALYSES OF WINE
257
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258 ANALYSIS OF ALCOHOLIC BEVERAGES
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Maximum
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ANALYSES OF CORDIALS AND LIQUEURS 259
tween 13 and 17. This is what is known as the acid: alcohol
ratio, and is used for the detection of watering. Water can be
added only to very sweet grapes without exceeding the limits of
this ratio and then only in very limited quantities.
The alcohol and extract vary directly and in such proportions
that the number representing the extract in grams per hundred
cc. multiplied by the factor 4.5 gives a figure equal to or greater
than the alcohol in grams per 100 cc. With white wines, in which
the extract is normally lower, the factor, 6.5 is used in the same
way. This is known as the alcohol: extract ratio and is used
for the detection of the addition of sugar to the must.
Analyses of Cordials and Liqueurs. As can be expected
from the wide range of proportions cited in Chapter XII for
making cordials their composition as shown by analysis also varies
greatly. However, Leach (loc. cit., p. 787) cites the following
results compiled by Konig as typical.
TABLE XXV. ANALYSES OF LIQUEURS.
Specific
gravity
Alcohol
by
volume
Alcohol
by
weight
Extract
Cane
sugar
Other
extrac-
tives
Ash
Absinthe
0.9116
C8.Q7
0.18
O. 72
Benedictine
.0700
<2.
78. c
76.00
72. C7
7 4.7
O O4.7
Ginger
.0481
47. c
76.0
27.70
2C.Q2
1.87
O I4.I
Crme de Menthe. . .
Anisette de Bordeaux
Curasao
.0447
.0847
.0700
48.0
42.0
cc.o
36.5
30.7
4.2. <
28.28
34.82
28.60
2 7 - 6 3
37-44
28. co
0.65
0.38
O. IO
0.068
O.040
o 040
Kummel
.0870
77. Q
24.8
72. 02
71.18
0.84
o.oc8
Angostura
O . Q C4.O
40. 7
<r.8c
4.16
I.6q
Chartreuse
I . O7QQ
47.18
76. ii
74. . 7 C
1.76
More generally these beverages may be classed according to
their sugar and alcohol content as follows :
TABLE XXVI.
Alcohol Sugar
Average grade 20-25% Io %
Good grade 25-30% 20%
Very good grade 30-40% 35%
Best grade 40-50% 45%
CHAPTER XIV
ANALYSIS OF ALCOHOLIC BEVERAGES
METHODS
(Reprinted by special permission from Official and Tentative Methods
of Analysis of the Association of Official Agricultural Chemists, 3rd ed.,
f930.)
WINES
I. PHYSICAL EXAMINATION TENTATIVE
Note and record the following: (i) Whether the container
is "bottle full"; (2) the appearance of the wine, whether it is
bright or turbid and whether there is any sediment; (3) con-
dition when opened, whether still, gaseous, or carbonated; (4)
color and depth of color; (5) odor, whether vinous, acetous,
pleasant, or foreign; and (6) taste, whether vinous, acetous,
sweet, dry, or foreign.
2. PREPARATION OF SAMPLE OFFICIAL
If gas is contained in the wine, remove it by pouring the
sample back and forth in beakers.
Filter the wine, regardless of appearance, before analyzing
and determine immediately the specific gravity and such ingredi-
ents as alcohol, acids, and sugars, which are liable to change
through exposure.
,3. SPECIFIC GRAVITY OFFICIAL
Determine the specific gravity at 20/4 (in vacuo) by means
of a pycnometer as follows: Carefully clean the pycnometer by
filling with a saturated solution of CrOs in H2&O4, allowing to
stand for several hours, emptying, and rinsing thoroughly with
H 2 O. Fill the pycnometer with recently boiled distilled H 2 O
260
ALCOHOL OFFICIAL 261
previously cooled to 16-18, place in a water bath cooled to the
same temperature and allow the bath to warm slowly to 20. Ad-
just the level of the H^O to the proper point on the pycnometer,
put the perforated cap or stopper in place, remove from the
bath ; wipe dry with a clean cloth, and after allowing to stand for
1520 minutes, weigh. Empty, rinse several times with alcohol
and then with ether, remove the ether fumes, allow the instrument
to become perfectly dry, and weigh. Ascertain the weight of
contained H2O at 20 in air (W of the formula below) by sub-
tracting the weight of the empty pycnometer from its weight when
full. Cool the sample to 16-18, adjust the level of the liquid to
the proper point on the pycnometer, put the perforated cap or
stopper in place, wipe dry, and weigh as before. Ascertain the
weight of the contained sample at 20 in air (S of the formula
below) by subtracting the weight of the empty pycnometer from
its weight when filled with the sample. Calculate the specific
gravity in vacuo by the following formula :
_, S -f . .
Q = - m which
1. 00282 W
G = corrected specific gravity of sample at 20/4 in vacuo ;
W = weight of contained H 2 O at 20 in air; and
S weight of contained sample at 20 in air.
4. ALCOHOL - OFFICIAL
(a) By volume. Measure 100 cc. of the liquid at 20 into
a 300-500 cc. distillation flask and add 50 cc. of H2O. Attach
the flask to a vertical condenser by means of a bent tube, distil
almost 100 cc., and make to a volume of 100 cc. at 20. (Foam-
ing, which sometimes occurs especially with young wines, may be
prevented by the addition of a small quantity of tannin.) To
determine the alcohol in wines that have undergone acetous fer-
mentation and contain an abormal quantity of acetic acid, exactly
neutralize the portion taken with NaOH solution before distilla-
tion. (This is unnecessary, however, for wines of normal taste
and odor.) Determine the specific gravity of the distillate at
2O/4 as directed under 3 and obtain the corresponding per-
centage of alcohol by volume from Tables A3-A5.
262 ANALYSIS OF ALCOHOLIC BEVERAGES
(b) Grams per 100 cc. From the specific gravity of the dis-
tillate, obtained under (a), ascertain the corresponding alcohol
content in g per 100 cc. from Tables AJ-A5.
(c) By weight. Divide the number of g in the 100 cc. of
distillate, as obtained in (b), by the weight of the sample as cal-
culated from its specific gravity.
(d) By immersion refractometer. Verify the percentages of
alcohol, as determined under (a) and (c), by ascertaining the
immersion refractometer reading of the distillate and obtaining
the corresponding percentages of alcohol from Table A6.
GLYCEROL IN DRY WINES
5. Method I (By Direct Weighing] Official
Evaporate 100 cc. of the wine in a porcelain dish on a water
bath to a volume of about 10 cc. Treat the residue with about
5 g. of fine sand and 45 cc. of milk of lime (containing 15 g.
of CaO per 100 cc.) for each g. of extract present and evaporate
almost to dryness. Treat the moist residue with 50 cc. of alcohol,
90% by volume; remove the substance adhering to the sides of
the dish with a spatula; and rub the whole mass to a paste.
Heat the mixture on a water bath, with constant stirring, to incip-
ient boiling and decant the liquid through a filter into a small flask.
Wash the residue repeatedly by decantation with 10 cc. portions of
hot 90% alcohol until the filtrate amounts to about 150 cc. Evap-
orate the filtrate to a sirupy consistency in a porcelain dish on
a hot, but not boiling, water bath; transfer the residue to a small
glass-stoppered, graduated cylinder with 20 cc. of absolute alco-
hol; and add 3 portions of 10 cc. each of anhydrous ether, shaking
thoroughly after each addition. Let stand until clear, pour off
through a filter, and wash the cylinder and filter with a mixture
of 2 parts of absolute alcohol to 3 parts of anhydrous ether, also
pouring the wash liquor through the filter. Evaporate the filtrate
to a sirupy consistency, dry for an hour at the temperature of
boiling H 2 O, weigh, ignite, and weigh again. The loss on ignition
gives the weight of glycerol.
REAGENTS 263
6. Method II (By Oxidation with Bichromate) Official
Evaporate 100 cc. of the wine in a porcelain dish on a water
bath, the temperature of which is maintained at 85-90, to a
volume of 10 cc. Treat the residue with about 5 g. of fine sand
and 5 cc. of milk of lime (containing 15 g. of CaO per 100 cc.).
Proceed from this point as directed under 7 and 8, beginning with
the clause "evaporate almost to dryness with frequent stirring,"
except to dilute the solution of glycerol after treatment with
(Ag 2 )CO3 and Pb-acetate to a volume of 100 cc. instead of
50 cc. Observe the precautions given concerning the temperature
at which all evaporations are to be made.
7. REAGENTS
(a) Strong potassium dichromate solution. Dissolve 74.55 g.
of dry, recrystallized K 2 Cr 2 O? in H2O; add 150 cc. of H 2 SO4;
cool; and dilute with H 2 O to I liter at 20 C. I cc. of this solu-
tion = 0.0 1 g. of glycerol. Owing to the high coefficient of expan-
sion of this strong solution it is necessary to make all volumetric
measurements of the solution at the same temperature as that at
which it was diluted to volume.
(b) Dilute potassium dichromate solution. Measure 25 cc.
of the strong K 2 Cr 2 O7 solution at 20 into a 500 cc. volumetric
flask and dilute to the mark with H 2 O at room temperature.
20 cc. of this solution = I cc. of (a).
(c) Ferrous ammonium sulfate solution. Dissolve 30 g. of
crystallized ferrous ammonium sulfate in H 2 O, add 50 cc. of
H 2 SO4, cool, and dilute with H 2 O to I liter at room temperature,
i cc. of this solution approximately I cc. of (b). As its value
changes slightly from day to day, it must be standardized against
(b) whenever used.
(d) Potassium ferricyanide indicator. Dissolve I g. of crys-
tallized K 3 Fe(CN) 6 in 50 cc. of H 2 O. This solution must be
freshly prepared.
(e) Milk of lime. Introduce 150 g. of CaO, selected from
clean hard lumps, prepared preferably from marble, into a large
264 ANALYSIS OF ALCOHOLIC BEVERAGES
porcelain or iron dish; slake with H^O, cool, and add sufficient
H2O to make i liter.
(f) Silver carbonate. Dissolve o.i g. of Ag2SO4 in about
50 cc. of H2O, add an excess of NagCOs solution, allow the
precipitate to settle, and wash with H2O several times by decanta-
tion until the washings are practically neutral. This reagent must
be freshly prepared immediately before use.
8. DETERMINATION
Make evaporations on a water bath maintained at a tempera-
ture of 85-90. The area of the dish exposed to the bath should
not be greater in circumference than that covered by the liquid
inside.
Evaporate 100 cc. of the vinegar to 5 cc., add 20 cc. of H2O,
and again evaporate to 5 cc. to expel acetic acid. Treat the
residue with about 5 g. of 4O-mesh sand and 15 cc. of the milk
of lime and evaporate almost to dryness, with frequent stirring,
avoiding the formation of a dry crust or evaporation to com-
plete dryness. Treat the moist residue with 5 cc. of H^O; rub
into a homogeneous paste; add slowly 45 cc. of absolute alcohol,
washing down the sides of the dish to remove adhering paste;
and stir thoroughly. Heat the mixture on a water bath, with
constant stirring, to incipient boiling; transfer to a suitable vessel;
and centrifugalize. Decant the clear liquid into a porcelain
dish and wash the residue with several small portions of hot
alcohol, 90% by volume, by aid of the centrifuge. (If a cen-
trifuge is not available, decant the liquid through a folded filter
into a porcelain dish. Wash the residue repeatedly with small
portions of hot 90% alcohol, twice by decantation, and then by
transferring all the material to the filter. Continue the washing
until the filtrate amounts to 150 cc.) Evaporate to a sirupy
consistency; add 10 cc. of absolute alcohol to dissolve this residue;
and transfer to a 50 cc. glass-stoppered cylinder, washing the dish
with successive small portions of absolute alcohol until the vol-
ume of the solution is 20 cc. Add 3 portions of 10 cc. each of
anhydrous ether, shaking thoroughly after each addition. Let
stand until clear, pour off through a filter, and wash the cylinder
DETERMINATION 265
and filter with a mixture of 2 volumes of absolute alcohol and 3
of anhydrous ether. If a heavy precipitate has formed in the
cylinder, centrifugalize at low speed, decant the clear liquid, and
wash 3 times with 20 cc. portions of the alcohol-ether mixture,
shaking the mixture thoroughly each time and separating the pre-
cipitate by means of the centrifuge. Wash the paper with the
alcohol-ether mixture and evaporate the filtrate and washings
on the water bath to about 5 cc., add 20 cc. of H^O, and again
evaporate to 5 cc. ; again add 20 cc. of H^O and evaporate to
5 cc.; finally add 10 cc. of H2O and evaporate to 5 cc.
These evaporations are necessary to remove all the ether and
alcohol, and when conducted at 85-90 they result in no loss of
glycerol if the concentration of the latter is less than 50%.
Transfer the residue with hot H^O to a 50 cc. volumetric
flask, cool, add the Ag2COs prepared from o.i g. of Ag 2 SC>4,
shake, and allow to stand 10 minutes. Then add 0.5 cc. of basic
Pb-acetate solution, shake occasionally, and allow to stand 10
minutes. Make up to the mark, shake well, filter, rejecting the
first portion of the filtrate, and pipet 25 cc. of the clear filtrate
into a 250 cc. volumetric flask.
Add i cc. of H2SO4 to precipitate the excess of Pb and then
30 cc. of Reagent (a). Add carefully 24 cc. of HfeSO^ rotating
the flask gently to mix the contents and avoid violent ebullition,
and then place in a boiling water bath for exactly 20 minutes.
Remove the flask from the bath, dilute, cool, and make up to the
mark at room temperature. The quantity of strong dichromate
solution used must be sufficient to leave an excess of about 12.5 cc.
at the end of the oxidation, the quantity given above (30 cc.)
being sufficient for ordinary vinegar containing about 0.35 g. or
less of glycerol per 100 cc.
Standardize the ferrous ammonium sulfate solution against
Reagent (b) by introducing from the respective burets approxi-
mately 20 cc. of each of these solutions into a beaker containing
100 cc. of H2O. Complete the titration, using Reagent (d) as
an outside indicator. From this titration calculate the volume (F)
of the ferrous ammonium sulfate solution equivalent to 20 cc.
of the dilute and therefore, to i cc. of Reagent (a).
266 ANALYSIS OF ALCOHOLIC BEVERAGES
In place of Reagent (b) solution substitute a buret containing
the oxidized glycerol with an excess of Reagent (a) and ascer-
tain how many cc. are equivalent to (F) cc. of the ferrous am-
monium sulfate solution and, therefore, to i cc. of Reagent (a).
Then 250, divided by this last equivalent, = the number of cc.
of Reagent (a) present in excess in the 250 cc. flask after oxida-
tion of the glycerol.
The number of cc. of Reagent (a) added, minus the excess
found after oxidation, multiplied by 0.02, gives the grams of
glycerol per 100 cc. of vinegar.
9. GLYCEROL IN SWEET WINES OFFICIAL
With wines in which the extract exceeds 5 g. per 100 cc.,
heat 100 cc. to boiling in a flask and treat with successive small
portions of milk of lime until the wine becomes first darker and
then lighter in color. Cool, add 200 cc. of 95% alcohol, allow
the precipitate to subside, filter, and wash with 95% alcohol.
Treat the combined filtrate and washings as directed under 5 or 6.
10. GLYCEROL-ALCOHOL RATIO OFFICIAL
Express this ratio as X : 100, in which X is obtained by multi-
plying the percentage weight of glycerol by 100 and dividing the
result by the percentage of alcohol by weight.
EXTRACT
ii. /. From the Specific Gravity of the Dealcoholized
Wine Official
Calculate the specific gravity of the dealcoholized wine by
the following formula:
S = G + i ~ A, in which
S = specific gravity of the dealcoholized wine;
G = specific gravity of the wine, 3 ; and
A = specific gravity of the distillate obtained in the determination of
alcohol, 4 (a).
From Table A2, ascertain the percentage by weight of extract
in the dealcoholized wine corresponding to the value of S. Mul-
REDUCING SUGARS OFFICIAL 267
tiply the figure thus obtained by the value of 5 to obtain the g.
of extract per 100 cc. of wine.
12. II. By Evaporation Official
(a) In dry wines, having an extract content of less than 3
grams per 100 cc. Evaporate 50 cc. of the sample on a water
bath to a sirupy consistency in a 75 cc. flat-bottomed Pt dish,
approximately 85 mm. in diameter. Heat the residue for 2-5
hours in a drying oven at the temperature of boiling H2O, cool in
a desiccator, and weigh as soon as the dish and contents reach
room temperature.
(b) In sweet wines. If the extract content is between 3 and
6 g. per 100 cc., treat 25 cc. of the sample as directed under (a).
If the extract exceeds 6 g. per 100 cc., however, the result, ob-
tained as directed under n, is accepted, and no gravimetric
determination is attempted because of the inaccurate results ob-
tained by drying levulose at a high temperature.
13. NON-SUGAR SOLIDS OFFICIAL
Determine the non-sugar solids (sugar- free extract) by sub-
tracting the quantity of reducing sugars before inversion, 14, from
the extract, n or 12. If sucrose is present in the wine, deter-
mine the nonsugar solids by subtracting the sum of reducing sugars
before inversion and the sucrose from the extract.
14. REDUCING SUGARS OFFICIAL
(a) Dry wines. Place 200 cc. of the wine in a porcelain dish;
exactly neutralize with normal NaOH, calculating the quantity
required from the determination of acidity, 44; and evaporate to
about Y$ the original volume. Transfer to a 200 cc. flask, add
sufficient neutral Pb-acetate solution to clarify, dilute to the mark
with H2O, shake, and pass through a folded filter. Remove the
Pb with dry K-oxalate and determine, reducing sugars as di-
rected under 1518.
(b) Sweet wines. With sweet wines, approximate the sugar
content by subtracting 2 from the result in the determination of
268 ANALYSIS OF ALCOHOLIC BEVERAGES
the extract and employ such a quantity of the sample that the
aliquot taken for the Cu reduction shall not exceed 240 mg. of
invert sugar. Proceed as directed under (a) except to take this
smaller quantity of the sample for the determination.
15. Munson and Walker General Method Official
REAGENTS
(a) Asbestos. Digest the asbestos, which should be the
amphibole variety, with HC1 (1+3) for 23 days. Wash free
from acid, digest for a similar period with 10% NaOH solu-
tion, and then treat for a few hours with hot alkaline tartrate
solution (old alkaline tartrate solutions that have stood for some
time may be used for this purpose) of the strength used in sugar
determinations. Wash the asbestos free from alkali; digest for
several hours with HNO 3 ( i + 3) ; and, after washing free from
acid, shake with H^O into a fine pulp. In preparing the Gooch
crucible, make a film of asbestos % i nc h thick and wash thor-
oughly with H2O to remove fine particles of asbestos. If the
precipitated Cu2O is to be weighed as such, wash the crucible
with 10 cc. of alcohol, then with 10 cc. of ether; dry for 30 minu-
utes at 100; cool in a desiccator; and weigh.
Soxhlet's modification of Fehlintfs solution. Prepared by
mixing immediately before use, equal volumes of (a) and (b).
(a) Copper sulfate solution. Dissolve 34.639 g. of
CuSO4.5H2O in H2O, dilute to 500 cc., and filter through pre-
pared asbestos.
(b) Alkaline tartrate solution. Dissolve 173 g. of Rochelle
salts and 50 g. of NaOH in H2O, dilute to 500 cc., allow to stand
for 2 days, and filter through prepared asbestos.
1 6. PRECIPITATION OF CUPROUS OXIDE
Transfer 25 cc. of each of the CuSO4 and alkaline tartrate
solutions to a 400 cc. beaker of alkali-resistant glass and add
50 cc. of the reducing sugar solution, or if a smaller volume of
sugar solution is used, add H2O to make the final volume 100 cc.
DETERMINATION 269
Heat the beaker on an asbestos gauze over a Bunsen burner, regu-
late the flame so that boiling begins in 4 minutes, and continue the
boiling for exactly 2 minutes. (It is important that these direc-
tions be strictly observed. To regulate the burner for this pur-
pose it is advisable to make preliminary tests, using 50 cc. of the
reagent and 50 cc. of H 2 O before proceeding with the actual
determination.) Keep the beaker covered with a watch-glass
during the heating. Filter the hot solution at once through an
asbestos mat in a porcelain Gooch crucible, using suction. Wash
the precipitate of Cu2O thoroughly with H 2 O at a temperature
of about 60 and either weigh directly as Cu 2 O as directed under
17, or determine the quantity of reduced Cu as described under
1 8. Conduct a blank determination, using 50 cc. of the reagent
and 50 cc. of H 2 O, and if the weight of Cu 2 O obtained exceeds
0.5 mg., correct the result of the reducing sugar determination
accordingly. The alkaline tartrate solution deteriorates on stand-
ing, and the quantity of Cu 2 O obtained in the blank increases.
iy. DETERMINATION OF REDUCED COPPER
Direct Weighing of Cuprous Oxide
(This method should be used only for determinations in solu-
tions of reducing sugars of comparatively high purity. In prod-
ucts containing large quantities of mineral or organic impurities,
including sucrose, determine the Cu of the Cu 2 O by one of the
methods described under 18, since the Cu 2 O is very likely to be
contaminated with foreign matter.)
Prepare a Gooch crucible as directed under 15. Collect the
precipitated Cu 2 O on the mat as directed under 16 and wash
thoroughly with hot H 2 O, then with 10 cc. of alcohol, and finally
with 10 cc. of ether. Dry the precipitate for 30 minutes in a
water oven at the temp, of boiling H 2 O, cool, and weigh. Calcu-
late the weight of metallic Cu, using the factor 0.8882. Obtain
from Table A7 the weight of invert sugar equivalent to the
weight of Cu.
The number of mg. of Cu reduced by a given quantity of
reducing sugar varies, depending upon whether or not sucrose is
270 ANALYSIS OF ALCOHOLIC BEVERAGES
present. In the tables the absence of sucrose is assumed except
in the entries under invert sugar, where, in addition to the column
for invert sugar alone, there are given one column for mixtures
of invert sugar and sucrose containing 0.4 g. of total sugar in
50 cc. of solution and one column for invert sugar and sucrose
when the 50 cc. of solution contains 2 g. of total sugar. Two
entries are also given under lactose and sucrose mixtures, showing
proportions of i part lactose to 4 and 12 parts of sucrose,
respectively.
1 8. REAGENTS
Volumetric Thiosulfate Method
Standard thiosulfate solution. Prepare a solution of
Na2S2Oa containing 19 g. of pure crystals in I liter. Weigh
accurately about 0.2 g. of pure Cu and place in a flask of 250 cc.
capacity. Dissolve by warming with 5 cc. of a mixture of equal
volumes of strong HNOs and H^O. Dilute to 50 cc., boil to
expel the red fumes, add a slight excess of strong Br water, and
boil until the Br is completely driven off. Cool, and add a strong
NaOH solution with agitation until a faint turbidity of Cu(OH)2
appears (about 7 cc. of a 25% NaOH solution is required). Dis-
charge the turbidity with a few drops of 80% acetic acid and add
2 drops in excess. (The solution should now occupy a volume of
50-70 cc.) Add 10 cc. of 30% KI solution. Titrate at once
with the thiosulfate solution until the brown tinge becomes weak
and add sufficient starch indicator to produce a marked blue
coloration. Continue the titration cautiously until the color
changes toward the end to a faint lilac. (If at this point the
thiosulfate is added dropwise and a little time is allowed for
complete reaction after each addition, no difficulty is experienced
in determining the end point within a single drop.) i cc. of the
thiosulfate solution = about 0.005 g. of Cu.
1 8a. DETERMINATION
After washing the precipitated Cu2O, cover the Gooch with
a watch-glass and dissolve the oxide by means of 5 cc. of warm
HNOs ( i + i ) poured under the watch-glass with a pipet. Col-
SUCROSE 271
lect the filtrate in a 250 cc. flask and wash the watch-glass and the
Gooch free from Cu, using about 50 cc. of F^O. Boil to expel
red fumes; add a slight excess of Br water; boil off the Br com-
pletely; and proceed as directed under 18, beginning with "Cool
and add a strong NaOH solution. . . ."
SUCROSE
19. /. By Reducing Sugars Before and After Inversion
Official
Determine the reducing sugars (clarification having been ef-
fected with neutral Pb-acetate, never with basic Pb-acetate) as
directed under 15 and calculate to invert sugar from Ay. Invert
the solution as directed under 20 (b) or (c), or 22 (b) or (c) ;
exactly neutralize the acid; and again determine the reducing
sugars, but calculate them to invert sugar from the table referred
to above, using the invert sugar column alone. Deduct the per-
centage of invert sugar obtained before inversion from that ob-
tained after inversion and multiply the difference by 0.95 to
obtain the percentage of sucrose. The solutions should be diluted
in both determinations so that not more than 240 mg. of invert
sugar is present in the quantity taken for reduction. It is im-
portant that all lead be removed from the solution with anhydrous
powdered K-oxalate or Na 2 CO 3 before reduction.
20. //. By Polarization Official
Polarize before and after inversion in a 200 mm. tube, as
directed under 20 or 22, a portion of the filtrate obtained under
14. In calculating the percentage of sucrose do not fail to take
into consideration the relation of the weight of the sample con-
tained in 100 cc. to the normal weight for the instrument.
(a) Direct reading. Pipet one 50 cc. portion of the Pb-free
filtrate into a 100 cc. flask, dilute with H 2 O to the mark, mix well,
and polarize in a 200 mm. tube. The result, multiplied by 2, is
the direct reading (P of formula given below) or polarization
before inversion. (If a 400 mm. tube is used, the reading
equals P.)
272 ANALYSIS OF ALCOHOLIC BEVERAGES
(b) Invert reading. First determine the quantity of acetic
acid necessary to render 50 cc. of the Pb-free filtrate distinctly
acid to methyl red indicator; then to another 50 cc. of the lead-
free solution in a 100 cc. volumetric flask, add the requisite quan-
tity of acid and 5 cc. of the invertase preparation, fill the flask
with H2O nearly to 100 cc., and let stand overnight (preferably
at a temperature not less than 20). Cool, and dilute to 100 cc.
at 20. Mix well and polarize at 20 in a 200 mm. tube. If
the analyst is in doubt as to the completion of the hydrolysis,
allow a portion of the solution to remain for several hours and
again polarize. If there is no change from the previous reading,
the inversion is complete, and the reading and temperature of the
solution should be carefully noted. If it is necessary to work at
a temperature other than 20, which is permissible within narrow
limits, the volumes must be completed and both direct and invert
readings must be made at the same temperature. Correct the
invert reading for the optical activity of the invertase solution
and multiply by 2. Calculate the percentage of sucrose by the
following formula:
100 (P - /) - .
S = ; 7 v T y m Which
142.1 + 0.073 (m 13) t/2
S = percentage of sucrose;
P = direct reading, normal soln. ;
/ = invert reading, normal soln. ;
/ = temp, at which readings are made ; and
m = g. of total solids in 100 cc. of the invert soln. read in the polariscope.
Determine the total solids as directed under n.
(c) Rapid inversion at 55-60. If more rapid inversion
is desired, proceed as follows: Prepare the sample as directed
under (a) and to 50 cc. of the Pb-free filtrate in a 100
cc. volumetric flask add glacial acetic acid in sufficient quan-
tity to render the solution distinctly acid to methyl red. The
quantity of acetic acid required should be determined before
pipetting the 50 cc. portion. Then add 10 cc. of invertase
solution, mix thoroughly, place the flask in a water bath at
55-60, and allow to stand at that temperature for 15 minutes
with occasional shaking. Cool, add Na2COs solution until dis-
SUCROSE 273
tinctly alkaline to litmus paper, dilute to 100 cc. at 20, mix
well, and determine the polarization at 20 in a 200 mm. tube.
Allow the solution to remain in the tube for 10 minutes and again
determine the polarization. If there is no change from the pre-
vious reading, the mutarotation is complete. Carefully note the
reading and the temperature of the solution. Correct the polar-
ization for the optical activity of the invertase solution and mul-
tiply by 2. Calculate the percentage of sucrose by the formula
given under (b).
(If the solution has been rendered so alkaline as to cause de-
struction of sugar, the polarization, if negative, will in general
decrease, since the decomposition of fructose ordinarily is more
rapid than that of the other sugars present. If the solution has
not been made sufficiently alkaline to complete mutarotation
quickly, the polarization, if negative, will in general increase. As
the analyst gains experience he may omit the polarization after
10 minutes if he has satisfied himself that he is adding Na2COs in
sufficient amount to complete mutarotation at once without caus-
ing any destruction of sugar during the period intervening before
polarization.)
21. //. By Polarization Before and After Inversion With
Hydrochloric Acid Official
(In the presence of much levulose, as in honeys, fruit prod-
ucts, sorghum sirup, cane sirup, and molasses, the optical method
for sucrose, requiring hydrolysis by acid, gives erroneous results.)
22. (a) Direct reading. Proceed as directed under 20 (a).
(b) Invert reading. Pipet a 50 cc. portion of the Pb-free
filtrate into a 100 cc. flask and add 25 cc. of H2O. Then add,
little by little, while rotating the flask, 10 cc. of HC1 (sp. gr.
1.1029 at 20/4 (or 24.85 Brix at 20)). Heat a water bath
to 70 and regulate the burner so that the temperature of the
bath remains approximately at that point. Place the flask in the
water bath, insert a thermometer, and heat with constant agita-
tion until the thermometer in the flask indicates 67. This pre-
liminary heating period should require from 2j^-2^ minutes.
274 ANALYSIS OF ALCOHOLIC BEVERAGES
From the moment the thermometer in the flask indicates 67,
leave the flask in the bath for exactly 5 minutes longer, during
which time the temperature should gradually rise to about 69.5.
Plunge the flask as once into Ir^O at 20. When the contents
have cooled to about 35, remove the thermometer from the
flask, rinse it, and fill almost to the mark. Leave the flask in the
bath at 20 for at least 30 minutes longer and finally make up
exactly to volume. Mix well and polarize the solution in a
200 mm. tube provided with a lateral branch and a water jacket,
maintaining a temperature of 20. This reading must also be
multiplied by 2 to obtain the invert reading. If it is necessary to
work at a temperature other than 20, which is permissible within
narrow limits, the volumes must be completed and both direct
and invert polarizations must be made at exactly the same temp.
Calculate sucrose by the following formula :
IPO (P - /) . . . ,
o : z~~z~7 \ 7~> in which
143 + 0.0676 (m 13) t/2
S = percentage of sucrose;
P = direct reading, normal soln. ;
I = invert reading, normal soln. ;
t = temp, at which readings are made; and
m = g. of total solids in 100 cc. of the invert soln. read in the polariscope.
Determine the total solids as directed under n.
(c) Inversion at room temperature. The inversion may
also be accomplished as follows: (i) To 50 cc. of the clarified
soln., freed from Pb, add 10 cc. of HC1 (sp. gr. 1.1029 at 20/4
or 24.85 Brix at 20) and set aside for 24 hours at a temp, not
below 20; or, (2) if the temp, is above 25, set aside for 10
hours. Make up to 100 cc. at 20 and polarize as directed under
(b). Under these conditions the formula must be changed to
the following:
100 (P - I)
n
143.2 + 0.0676 (m 13) - t/2
23. COMMERCIAL GLUCOSE OFFICIAL
Polarize a portion of the clarified filtrate after inversion in a
200 mm. jacketed tube at 87, as directed under 24. In calcu-
ASH EXTRACT RATIO OFFICIAL 275
lating the percentage of glucose do not fail to take into con-
sideration the relation of the weight of the sample contained in
100 cc. to the normal weight for the instrument.
24. Commercial glucose cannot be determined accurately ow-
ing to the varying quantities of dextrin, maltose, and dextrose
present in the product. However, in sirups in which the quantity
of invert sugar is so small as not to affect appreciably the result,
commercial glucose may be estimated approximately by the fol-
lowing formula :
(a-S) IPO . , . ,
Q in w hich
211
G = percentage of commercial glucose solids;
a = direct polarization, normal soln.; and
S = percentage of cane sugar.
Express the results in terms of commercial glucose solids polariz-
ing + 21 iV. (This result may be recalculated in terms of com-
mercial glucose of any Baume reading desired.)
25. ASH OFFICIAL
Proceed as directed below using the residue from 50 cc. of
the wine.
Weigh a quantity of the substance representing about 2 g.
of dry material and burn at a low heat, not exceeding dull red-
ness, until free from C. If a C-free ash cannot be obtained in
this manner, exhaust the charred mass with hot H2O, collect the
insoluble residue on an ashless filter, and burn the filter and con-
tents to a white or nearly white ash. Add the filtrate, evaporate
to dryness, and heat at dull redness until the ash is white or
grayish white. Cool in a desiccator and weigh.
26. ASH EXTRACT RATIO OFFICIAL
Express results as i : X, in which X is the quotient obtained by
dividing the g. of extract per 100 cc. by the g. of ash per 100 cc.
276 ANALYSIS OF ALCOHOLIC BEVERAGES
27. ALKALINITY OF THE WATER-SOLUBLE ASH OFFICIAL
Extract the ash obtained as directed under 25 with successive
small portions of hot H 2 O until the filtrate amounts to about
60 cc.
Cool the filtrate and titrate with o.i N HC1, using methyl
orange indicator. Express the alkalinity in terms of the num-
ber of cc. of o.i N acid per 100 cc. of the wine.
28. ALKALINITY OF THE WATER-INSOLUBLE ASH OFFICIAL
Ignite the filter and residue from 27 in the Pt. dish in which
the wine was ashed and proceed as directed below. Express the
alkalinity in terms of the number of cc. of o.i N acid required
to neutralize the water-insoluble ash from 100 cc. of the wine.
Add an excess of o.i N HC1 (usually 10-15 cc.) to the
ignited insoluble ash in the Pt. dish, heat to boiling on an as-
bestos plate, cool, and titrate the excess of HC1 with o.i N
NaOH, using methyl orange indicator.
29. PHOSPHORIC ACID OFFICIAL
Dissolve the ash obtained as directed under 25 in 50 cc. of
boiling HNOs (1+9), filter, wash the filter, and determine
P 2 Os in the combined filtrate and washings as directed below.
If the ash ignites without difficulty, no free phosphoric acid need
be suspected. Should there be any free acid, the ash remains
black even after repeated leaching. In such cases, add Ca-ace-
tate or a mixture containing 3 parts of Na2COs and i part of
NaNOs to avoid loss of P^O^ before attempting to ash. Add
NHUOH in slight excess; and barely dissolve the precipitate
formed with a few drops of HNOs, stirring vigorously. If HC1
or H2&O4 has been used as a solvent, add about 15 g. of crys-
talline NH4NOs or a soln. containing that quantity. To the hot
soln. add 70 cc. of molybdate soln. for every decigram of P2Os
.present. Digest at about 65 for i hour, and determine whether
or not the P2Os has been completely precipitated by the addition
of more molybdate soln. to the clear supernatant liquid. Filter,
CHLORIDES OFFICIAL 277
and wash with cold H 2 O or preferably with the NH 4 NO 3 soln.
Dissolve the precipitate on the filter with NIHUOH (i + i) and
hot H 2 O and wash into a beaker to a volume of not more than
100 cc. Neutralize with HC1, using litmus paper or bromthy-
mol blue as an indicator; cool; and from a buret add slowly (about
i drop per second), stirring vigorously, 15 cc. of magnesia mix-
ture for each decigram of P 2 Os present After 15 min. add
12 cc. of NHUOH. Let stand until the supernatant liquid is
clear (usually 2 hours), filter, wash the precipitate with the
dilute NHUOH until the washings are practically free from
chlorides, dry, burn first at a low heat and ignite to constant
weight, preferably in an electric furnace, at 950-1,000; cool
in a desiccator, and weigh as Mg2P2O7. Calculate and report
the result as percentage of P 2 Os.
30. SULFURIC ACID OFFICIAL
Precipitate directly the H 2 SO4 in 50 cc. of the wine by means
of 10% BaCl 2 soln. after acidifying with a small excess of HC1,
and determine the resulting BaSO4 as directed below. Allow the
precipitate to stand for at least 6 hours before filtering. Report
as SOs, using the factor 0.3430.
Heat to boiling and add slowly in small quantities a 10%
BaCl 2 soln. until no further precipitate is formed. Continue the
boiling for about 5 min. and allow to stand for 5 hours or longer
in a warm place. Decant the liquid through an ashless filter or an
ignited and weighed Gooch crucible, treat the precipitate with
15-20 cc. of boiling H 2 O, transfer to the filter, and wash with
boiling H 2 O until the filtrate is free from chlorides. Dry the
precipitate and filter, ignite, and weigh as BaSO4.
3 I . CHLORIDES OFFICIAL
To 100 cc. of dry wine or 50 cc. of sweet wine, add sufficient
Na 2 COs to make distinctly alkaline. Evaporate to dryness, ignite
at a heat not above low redness, cool, extract the residue with
hot H 2 O, acidify the water extract with HNO 3 (i +4)
determine chlorides as directed under 32 or 34.
278 ANALYSIS OF ALCOHOLIC BEVERAGES
32. /. Gravimetric Method
To the soln. prepared as directed in 31 add a IQ% AgNO 3
soln., avoiding more than a slight excess. Heat to boiling, pro-
tect from the light, and allow to stand until the precipitate is
granular. Filter on a weighed Gooch crucible, previously heated
to 140-150, and wash with hot H2O, testing the filtrate to prove
excess of AgNO 3 . Dry the AgCl at 140-150, cool, and weigh.
Report as percentage of Cl.
33. //. Volumetric Method
REAGENTS
(a) Silver nitrate. Adjust to exact Q.I N strength by stand-
ardizing against a o.i N NaCl soln. containing 5.846 g. of pure
NaCl per liter.
(b) Ammonium or potassium thiocyanate. o.i N. Adjust
by titrating against the o.i N AgNOs.
(c) Ferric indicator. A saturated soln. of ferric ammonium
alum.
(d) Nitric acid. Free from lower oxides of N by diluting
the usual pure acid with about J4 volume of HoO, and boiling
until perfectly colorless.
34. DETERMINATION
To the soln. prepared as directed under 31, add a known
volume of the o.i N AgNOs in slight excess. Stir well, filter, and
wash the AgCl precipitate thoroughly. To the combined filtrate
and washings add 5 cc. of the ferric indicator and a few cc. of
the HNOs and titrate the excess of Ag with the o.i N thiocy-
anate until a permanent light brown color appears. From the
number of cc. of o.i N AgNOs used, calculate the quantity of Cl.
i cc. of o.i TV AgNO 3 = 0.003 5 5 g. of Cl.
35. TOTAL ACIDS OFFICIAL
Measure 20 cc. of the wine into a 250 cc. beaker, heat rapidly
to incipient boiling, and immediately titrate with o.i N NaOH
VOLATILE ACIDS 279
soln. Determine the end point with neutral 0.05% azolitmin
soln. as an outside indicator. Place the indicator in the cavities
of a spot plate and spot the wine into the azolitmin soln. The
end point is reached when the color of the indicator remains un-
changed by the addition to the wine of a few drops of o.i N
alkali.
In the case of wines that are artificially colored and therefore
cannot be titrated satisfactorily in the above manner, it will be
found helpful to use phenolphthalein powder (one part of phe-
nolphthalein mixed with 100 parts of dry, powdered K2SO4) as
an indicator. Place this indicator in the cavities of a spot plate
and spot the wine into the powder. The end of the titration is
indicated when the powder acquires a pink tint.
Express the result in terms of tartaric acid. I cc. of o.i N
NaOH soln. = 0.0075 g- f tartaric acid.
VOLATILE ACIDS
36. Method I Official
Heat rapidly to incipient boiling 50 cc. of the wine in a 500
cc. distillation flask and pass steam through until 15 cc. of the dis-
tillate requires only 2 drops of o.i N NaOH soln. for neutraliza-
tion. Boil the H2O used to generate the steam several minutes
before connecting the steam generator with the distillation flask
in order to expel CO2. Titrate rapidly with o.i N NaOH soln.,
using phenolphthalein indicator. The color should remain about
10 seconds. Express the result as acetic acid. I cc. of o.i TV
NaOH soln. = 0.0060 g. of acetic acid.
37. Method II Official
Introduce 10 cc. of the wine, previously freed from CO2, into
the inner tube of a modified Sellier distillation apparatus (Fig.
50) ; add a small piece of paraffin to prevent foaming; and adjust
the tube and its contents in place within the larger flask, which
contains 100 cc. of recently boiled H2O. Connect with a con-
denser as illustrated in the figure and distil by heating the outer
280 ANALYSIS OF ALCOHOLIC BEVERAGES
flask. When 50 cc. of the distillate has been collected, empty
the receiver into a beaker and titrate with o.i N NaOH soln.,
using phenolphthalein indicator. Continue the distillation and
titrate each succeeding 10 cc. of distillate until not more than i
drop of standard alkali is required to reach the neutral point.
Usually 80 cc. of distillate will contain all the volatile acids.
FIG. 50.
38. FIXED ACIDS OFFICIAL
To obtain the quantity of fixed acids, expressed as tartaric
acid, multiply the quantity of volatile acids by 1.25 and subtract
this product from the total acids.
39. TOTAL TARTARIC ACID OFFICIAL
Neutralize 100 cc. of the wine with A^ NaOH soln., calcu-
lating from the acidity, 44, the number of cc. o/ TV alkali neces-
sary for the neutralization. If the volume of the soln. is increased
more than 10% by the addition of the alkali, evaporate to ap-
proximately 100 cc. Add to the neutralized soln. 0.075 ^
tartaric acid for each cc. of TV alkali added and after the tartaric
acid has dissolved add 2 cc. of glacial acetic acid and 15 g. of
KC1. After the KC1 has dissolved, add 15 cc. of 95% alcohol;
stir vigorously until the K-bitartrate begins to precipitate; and let
stand in an ice-box at 15-18 for at least 15 hours. Decant the
liquid from the separated K-bitartrate on a Gooch crucible pre-
pared with a very thin film of asbestos, or on filter paper in a
TANNIN AND COLORING MATTER 281
Biichner funnel. Wash the precipitate and filter 3 times with a
few cc. of a mixture of 15 g. of KC1, 20 cc. of 95% alcohol, and
100 cc. of H2O, using not more than 20 cc. of the wash soln. in
all. Transfer the asbestos or paper and precipitate to the
beaker in which the precipitation was made; wash the Gooch
crucible or Biichner funnel with hot H2O, using about 50 cc.
in all; heat to boiling; and titrate the hot soln. with o.i N NaOH
soln., using phenolphthalein indicator. Increase the number of
cc. of o.i N alkali required by 1.5 cc. to allow for the solubility
of the precipitate. I cc. of o.i N alkali is equivalent, under these
conditions, to 0.015 g. of tartaric acid. To obtain the g. of total
tartaric acid per 100 cc. of the wine, subtract the quantity of
tartaric acid added from this result.
40. FREE TARTARIC ACID AND CREAM OF TARTAR OFFICIAL
Calculate the free tartaric acid and cream of tartar in the
following manner:
Let A = total tartaric acid in 100 cc. of wine, divided by 0.015;
B = total alkalinity of the ash (sum of C and D) ;
C = alkalinity of water-soluble ash ; and
D = alkalinity of water-insoluble ash.
Then
( i ) If A is greater than B f
Cream of tartar = 0.0188 X C, and
Free tartaric acid = 0.015 X (A ~ B) ;
(2) If A equals B or is smaller than B but greater than C
Cream of tartar = 0.0188 X C, and
Free tartaric acid = o; and
(3) If A is smaller than C,
Cream of tartar = 0.0188 X A, and
Free tartaric acid = o.
41. TANNIN AND COLORING MATTER OFFICIAL
REAGENTS
(a) Oxalic acid. o.i N. I cc. = 0.00416 g. of tannin.
(b) Standard potassium permanganate soln. Dissolve
1.333 g. of KMnO 4 in i liter of H2O and standardize the soln.
against (a).
282 ANALYSIS OF ALCOHOLIC BEVERAGES
(c) Indigo soln. Dissolve 6 g. of Na-sulfindigotate in 500
cc. of H2O by heating, cool, add 50 cc. of H 2 SO4, make up to i
liter, and filter.
(d) Purified boneblack. Boil 100 g. of finely powdered
boneblack with successive portions of HC1 (4-3), filter, and
wash with boiling H 2 O until free from chlorides. Keep covered
with H 2 O.
42. DETERMINATION
Dealcoholize 100 cc. of the wine by evaporation and dilute
with H2O to the original volume. Transfer 10 cc. to a 2-liter
porcelain dish and add about I liter of H 2 O and exactly 20 cc.
of the indigo soln. Add the standard KMnO4 soln., i cc. at a
time, until the blue color changes to green; then add a few drops
at a time until the color becomes golden yellow. Designate the
number of cc. of KMnO4 soln. used as "a."
Treat 10 cc. of the dealcoholized wine, prepared as above,
for 15 min. w r ith boneblack; filter; and wash thoroughly with
H 2 O. Add i liter of H 2 O and 20 cc. of the indigo soln. and
titrate with KMnO-i, as above. Designate the number of cc. of
KMnO 4 used as "b."
Then a b c, the number of cc. of the KMnO4 soln. re-
quired for the oxidation of the tannin and coloring matter in 10
cc. of the wine.
43. CRUDE PROTEIN OFFICIAL
Determine N in 50 cc. of the wine as directed below, and
multiply the result by 6.25.
Place the sample in a digestion flask. Add approximately
0.7 g. of HgO, or its equivalent in metallic Hg, and 20-30 cc.
of H 2 SO4 (0.1-0.3 g. of crystallized CuSO4 may also be used
in addition to the Hg, or in many cases, in place of it). Place
the flask in an inclined position and heat below the boiling point
of the acid until frothing has ceased. (A small piece of paraffin
may be added to prevent extreme foaming.) Increase the heat
until the acid boils briskly and digest for a time after the mixture
REAGENTS 283
is colorless or nearly so, or until oxidation is complete. (The
digestion usually requires at least 2 hours.)
After cooling, dilute with about 200 cc. of H 2 O, and add a
few pieces of granulated Zn or pumice stone to prevent bumping,
and 25 cc. of K 2 S or Na 2 S 2 O 3 soln. with shaking. (If Na 2 S 2 O 3
is to be used, it should first be mixed with the NaOH so that they
may be added together. When no Hg or HgO is used the addi-
tion of K 2 S or Na 2 S or Na 2 S 2 O 3 soln. is unnecessary.) Next add
sufficient NaOH soln. to make the reaction strongly alkaline (50
cc. is usually sufficient), pouring it down the side of the flask
so that it does not mix at once with the acid soln. Connect the
flask to the condenser by means of a Kjeldahl connecting bulb,
taking care that the tip of the condenser extends below the sur-
face of the standard acid in the receiver; mix the contents by
shaking; and distil until all NH 3 has passed over into a measured
quantity of the standard acid. (The first 150 cc. of the distillate
will generally contain all the NH 3 .) Titrate with standard alkali
soln., using the methyl red or cochineal indicator.
44. PENTOSANS OFFICIAL
Proceed as directed under 45, 46, except to use 100 cc. of the
wine and 43 cc. of HC1 in beginning the distillation. Owing to
the interference of sugars this determination can be made in dry
wines only.
45. REAGENTS
(a) Hydrochloric acid. Contains 12% by weight HC1. To
i volume of HC1 add 2 volumes of H 2 O. Determine the per-
centage of acid by titration against standard alkali and adjust to
proper strength by dilution or addition of more strong acid, as
may be necessary.
(b) Phloroglucin. Dissolve a small quantity of phloro-
glucin in a few drops of acetic anhydride, heat almost to boiling,
and add a few drops of H 2 SO 4 . A violet color indicates the
presence of diresorcin. A phloroglucin which gives more than a
faint coloration may be purified by the following method :
284 ANALYSIS OF ALCOHOLIC BEVERAGES
Heat in a beaker about 300 cc. of the dilute HC1 (a) and
1 1 g. of commercial phloroglucin, added in small quantities at a
time, stirring constantly until it is nearly dissolved. Pour the
hot soln. into a sufficient quantity of the same HC1 (cold) to make
the volume 1500 cc. Allow to stand at least over night, prefer-
ably several days, to permit the diresorcin to crystallize. Filter
immediately before using. A yellow tint does not interfere with
its usefulness. In using, add the volume containing the required
quantity of phloroglucin to the distillate.
46. DETERMINATION
Place the sample in a 300 cc. distillation flask, together with
100 cc. of the dilute HC1 and several pieces of recently ignited
pumice stone. Place the flask on a wire gauze; connect with a
condenser; and heat, rather gently at first, but then regulating
so as to distil over 30 cc. in about 10 min. Pass the distillate
through a small filter paper. Replace the 30 cc. distilled by a like
quantity of the dilute acid, added by means of a separatory fun-
nel in such a manner as to wash down the particles adhering to
the sides of the flask, and continue the process until the distillate
amounts to 360 cc. To the total distillate add gradually a
quantity of phloroglucin dissolved in the dilute HC1 and thor-
oughly stir the resulting mixture. The quantity of phloroglucin
used should be about double that of the furfural expected. The
soln. turns yellow, then green, and very soon there appears an
amorphous greenish precipitate that grows darker rapidly, till it
becomes almost black. Make the soln. up to 400 cc. with the
dilute HC1 and allow to stand over night.
Collect the amorphous black precipitate in a weighed Gooch
crucible having an asbestos mat, wash carefully with 150 cc. of
H 2 O so that the H 2 O is not entirely removed from the crucible
until the very last, then dry for 4 hours at the temp, of boiling
H2O, cool, and weigh in a weighing bottle. The increase in
weight is taken to be furfural phloroglucide. To calculate the
furfural, pentose, or pentosan from the phloroglucide, use the
following formulas given by Krober:
GUM AND DEXTRIN TENTATIVE 285
1 i ) For a weight of phloroglucide, designated by "a" in the following
formulas, under 0.03 g,
Furfural = (a + 0.0052) X 0.5170.
Pentoses = (a + 0.0052) X 1.0170.
Pentosans = (a + 0.0052) X 0.8949.
In the above and also in the following formulas, the factor 0.0052 rep-
resents the weight of the phloroglucide that remains dissolved in the 400
cc. of acid soln.
(2) For a weight of phloroglucide "a" between 0.03 and 0.300 g., use
the following formulas:
Furfural = (a + 0.0052) X 0.5185.
Pentoses = (a + 0.0052) X 1.0075.
Pentosans = (a + 0.0052) X 0.8866.
(3) For a weight of phloroglucide "ct* over 0.300 g.,
Furfural = (a + 0.0052) X 0.5180.
Pentoses = (a + 0.0052) X 1.0026.
Pentosans = (a + 0.0052) X 0.8824.
47. GUM AND DEXTRIN TENTATIVE
Evaporate 100 cc. of the wine to about 10 cc. and add 10 cc.
of 95% alcohol. If gum or dextrin is present (indicated by the
formation of a voluminous precipitate), continue the addition of
alcohol, slowly and with stirring, until 100 cc. has been added.
Let stand over night; filter; and wash with alcohol, 80% by vol-
ume. Dissolve the precipitate on the paper with hot H 2 O, hydro-
lyze the filtrate and washings with HC1, and proceed as directed
below.
48. (This method is intended only for such materials as raw
starch, potatoes, etc., and includes as starch the pentosans and
other carbohydrate bodies that undergo hydrolysis and are con-
verted into reducing sugars on boiling with HC1.)
49. Heat the liquid for 2.5 hours with 200 cc. of H 2 O and
20 cc. of HC1 (sp. gr. 1.125) * n a fl as ^ provided with a reflux
condenser. Cool, and nearly neutralize with NaOH. Complete
the volume to 250 cc., filter and determine the dextrose in an
aliquot of the filtrate as directed under 16 and 17 or 18. The
weight of the dextrose obtained multiplied by 0.90 gives the
weight of starch.
286 ANALYSIS OF ALCOHOLIC BEVERAGES
50. NITRATES TENTATIVE
(a) White wine. Treat a few drops of the wine in a por-
celain dish with 2-3 cc. of H2SO4 that contains about o.i g. of
diphenylamine per 100 cc. The deep blue color formed in the
presence of nitrates appears so quickly that it is not obscured,
even in sweet wine, by the blackening produced by the action of
H2SO4 on the sugar.
(b) Red wine. Clarify with basic lead acetate, filter, re-
move the excess of Pb from the filtrate with Na2$O4, filter again,
and treat a few drops of this filtrate as directed under (a).
5 I . COLORING MATTERS AND PRESERVATIVES
These subjects are treated extensively in Chapters XXI and
XXXII of the Official and Tentative Methods of Analysis of the
Association of Official Agricultural Chemists, 3rd ed. 1930,
to which the student is referred. The following note is applicable
to the question of preservatives in wine.
The detection of added boric acid is somewhat difficult be-
cause a small quantity of it is normally present in certain wines.
Therefore a quantitative determination should be made. The
determination of SO2 must also be quantitative. A small quantity
of salicylic acid is also normal in wine, and for that reason not
more than 50 cc. of the sample should be used in testing for that
preservative.
DISTILLED LIQUORS
52. SPECIFIC GRAVITY OFFICIAL
Determine the specific gravity at 20/4 by means of a pycnom-
eter, as directed under 3, or by means of a small, accurately
graduated hydrometer.
53. ALCOHOL RY WEIGHT OFFICIAL
Weigh 20-25 g. of the sample into a distillation flask, dilute
with 100 cc. of H2O, and distil nearly 100 cc. Weigh the dis-
tillate or make to volume at 20, In either case determine the
ASH OFFICIAL 287
specific gravity as directed under 3. Obtain the corresponding
percentage of alcohol by weight from Tables A3-A5 ; multiply
this figure by the weight of the distillate; and divide by the weight
of the sample taken to obtain the percentage of alcohol by weight.
The alcohol content of the distillate may be checked by deter-
mining the immersion refractometer reading and obtaining the
percentage of alcohol from Table A6.
ALCOHOL BY VOLUME
54. Method I Official
From the specific gravity of the distillate obtained under 53
ascertain the corresponding percentage of alcohol by volume from
Tables A3-A5. Multiply this figure by the volume of distillate
and divide by the volume of the sample (calculated from the
specific gravity) to obtain the percentage of alcohol by volume
in the original sample.
55. Method II Official
Measure 25 cc. of the sample at 20 into a distillation flask,
dilute with 100 cc. of H^O, distil nearly 100 cc., make to volume
at 20, and determine the specific gravity as directed under 53.
Obtain, from Tables A3-A5, the corresponding percentage of
alcohol by volume in the distillate and multiply by 4 to obtain the
percentage of alcohol by volume in the original substance.
The alcohol content of the distillate may be checked by de-
termining the immersion refractometer reading and obtaining the
percentage of alcohol from Table A6.
5 6. EXTRACT OFFICIAL
Weigh, or measure at 20, 100 cc. of the sample, evaporate
nearly to dryness on a steam bath, transfer to a water oven, and
dry at the temp, of boiling FbO for 2.5 hours.
57. ASH OFFICIAL
Proceed as directed under 25 using the residue from the de-
termination of the extract c6.
288 ANALYSIS OF ALCOHOLIC BEVERAGES
58. ACIDITY OFFICIAL
Titrate 100 cc. of the sample (or 50 cc. diluted to 100 cc. if
the sample is dark) with o.i N alkali, using phenolphthalein in-
dicator. Express the result as acetic acid. I cc. of o.i N alkali
= 0.0060 g. of acetic acid.
59. ESTERS OFFICIAL *
Measure 100200 cc. of the sample into a distillation flask;
add 12.5-25 cc. of H2O; and distil slowly 100-200 cc., depend-
ing upon the amount of sample taken, using a mercury valve to
prevent loss of alcohol. Exactly neutralize the free acid in 50
cc. of the distillate with o.i N alkali and add a measured excess
of 2550 cc. of o.i TV alkali. Then either boil for an hour under
a reflux condenser, cool, and titrate with o.i TV acid, or allow
the soln. to stand over night in a stoppered flask with the excess
of alkali, heat with a tube condenser for 30 min. at a temp, below
the boiling point, cool, and titrate. Calculate the number of cc.
of o.i TV alkali used in the saponification of the esters as ethyl
acetate, i cc. of o.i N alkali = 0.0088 g. of ethyl acetate. Run
a blank, using water in place of the distillate, and make any neces-
sary correction.
60. ALDEHYDES OFFICIAL
REAGENTS
(a) Aldehyde-free alcohol. Redistil 95% alcohol over
NaOH or KOH; add 23 g. per liter of meta-phenylenediamine
hydrochloride ; digest at ordinary temp, for several days (or
under a reflux condenser on a steam bath for several hours) ; and
distil slowly, rejecting the first 100 cc. and the last 200 cc. of the
distillate.
(b) Sulfite-fuchsln soln. Dissolve 0.50 g. of pure fuchsin
in 500 cc. of H2O, add 5 g. of SO2 dissolved in H^O, make up
to i liter, and allow to stand until colorless. As this soln. decom-
poses rapidly, prepare it in small quantities and keep at a low
temp.
*The use of "100-200 cc." instead of "200 cc." and of "12.5-25 cc." instead of
"25 cc." has been approved as official, first action.
DETERMINATION 289
(c) Standard acetaldehyde so In. Prepare according to the
directions of Vasey, as follows: Grind aldehyde ammonia in a
mortar with anhydrous ether and decant the ether. Repeat this
operation several times and dry the purified salt in a current of
air and then in vacuo over H^SO,*. Dissolve 1.386 g. of this
purified aldehyde ammonia in 50 cc. of 95% alcohol, add 22.7
cc. of N alcoholic H 2 SO 4 , make up to 100 cc. and add 0.8 cc. of
alcohol for the volume of the (NH4) 2 SO 4 precipitate. Allow
the mixture to stand over night, and filter. This soln. contains i g.
of acetaldehyde in 100 cc. and will retain its strength.
The standard found most convenient for use is 2 cc. of this
strong aldehyde soln. diluted to 100 cc. with alcohol, 50% by vol-
ume, i cc. of this soln. = 0.0002 g. of acetaldehyde. Make up
the soln. every day or so, as it loses strength.
6 1 . DETERMINATION
Determine the aldehyde in the distillate prepared as directed
under 65. Dilute 5-10 cc. of the distillate to 50 cc. with alde-
hyde-free alcohol, 50% by volume; add 25 cc. of the sulfite-
fuchsin soln.; and allow to stand for 15 min. at 15. The solns.
and reagents should be at 15 when they are mixed. Prepare
standards of known strength and blanks in the same way. The
comparison standards found most convenient for use contain o.i,
0.2, 0.3, 0.4, 0.5, and 0.6 mg. of acetaldehyde.
62. FURFURAL OFFICIAL
REAGENT
Standard furfural soln. Dissolve i g. of redistilled furfural
in 100 cc. of 95% alcohol. Prepare standards by diluting I cc.
of this soln. to 100 cc. with alcohol, 50% by volume, i cc. of
this soln. contains o.i mg. of furfural. (The strong furfural soln.
will retain its strength, but the dilute soln. will not.)
63. DETERMINATION
Dilute 10-20 cc. of the distillate, as prepared under 65, to
to cc. with furfural-free alcohol, 50% by volume. Add 2 cc. of
2 9 o ANALYSIS OF ALCOHOLIC BEVERAGES
colorless aniline and 0.5 cc. of HC1 (sp. gr. 1.125) an d keep
for 15 min. in a water bath at about 15. Prepare standards of
known strength and blanks in the same way. The comparison
standards found most convenient for use contain 0.05, o.i, 0.15,
0.2, 0.25, and 0.3 mg. of furfural.
64. FUSEL OIL - OFFICIAL*
REAGENTS
(a) Purified carbon tctrachloride. Mix in a separatory
funnel crude CCU with I /IQ its volume of H^SO^ shake thoroughly
at frequent intervals, and allow to stand overnight. Wash free
of acid and impurities with tap H^O, remove the HkO, add an
excess of NaOH soln., and distil the CCU.
The refuse CCU after titration is purified for further work
by collecting in a large bottle, adding NaOH soln. ( i -f i ), shak-
ing, washing with tap H2O until the washings are neutral to
phenolphthalein, and distilling.
(b) Oxidizing soln. Dissolve 100 g. of K^C^Oy in 900 cc.
of H2O and add 100 cc. of
65. DETERMINATION
(i) To 50 cc. of the sample add 50 cc. of H^O, then add
20 cc. of 0.5 N NaOH, and saponify the mixture by boiling for
an hour under a reflux condenser; or, (2) mix 50 cc. of the liquid
and 50 cc. of H2O with 20 cc. of 0.5 N NaOH, allow to stand
overnight at room temp., and distil directly. Connect the flask
with a distillation apparatus, distil 90 cc., add 25 cc. of H2O,
and continue the distillation until an additional 25 cc. is collected.
Whenever aldehydes are present in excess of 15 parts per
100,000, add to the distillate 0.5 g. of metaphenylenediamine
hydrochloride, boil under a reflux condenser for an hour, distil
100 cc., add 25 cc. of H2O, and continue the distillation until
an additional 25 cc. is collected.
*In 65, lines i and 3, the use of "50 cc." instead of "100 cc." has been approved
as official, first action.
METHYL ALCOHOL 291
Approximately saturate the distillate with finely ground NaCl
and add saturated NaCl soln. until the specific gravity is i.io.
Extract this salt soln. 4 times with the purified CCU, using
40, 30, 20, and 10 cc., respectively, and wash the CCL* .3 times
with 50 cc. portions of saturated NaCl soln., and twice with satu-
rated Na2SO4 soln. Transfer the CCU to a flask containing 50
cc. of the oxidizing soln. and boil for 8 hours under a reflux
condenser.
Add 100 cc. of H2O and distil until only about 50 cc. remains.
Add 50 cc. of H2O and again distil until 35-50 cc. is left. Use
extreme care to prevent the oxidizing mixture from burning and
baking on the side of the distilling flask. The distillate should
be water white; if it is colored discard it and repeat the deter-
mination. Titrate the distillate with o.i N NaOH, using phenol-
phthalein indicator, i cc. of o.i N NaOH = 0.0088 g. of amyl
alcohol.
If preferred, use rubber stoppers in the saponification and first
distillation, but use corks covered with tinfoil in the oxidation
and second distillation. Renew the corks and tinfoil frequently.
Conduct a blank determination upon 100 cc. of CCU, begin-
ning the blank at that point of the procedure immediately after
the extraction and just before the washings with NaCl and
Na2SO4 solns.
66. SUGARS OFFICIAL
Proceed as directed under 14-24.
METHYL ALCOHOL
67. Trillat Method Official
To 50 cc. of the sample add 50 cc. of H2O and 8 g. of lime
and fractionate by the aid of Glinsky bulb tubes. Dilute the first
15 cc. of the distillate to 150 cc., mix with 15 g. of K^Cr^O? and
70 cc. of H2SO4 ( i + 5), and allow to stand for i hour, shaking
occasionally.
Distil, reject the first 25 cc., and collect 100 cc. Mix 50 cc.
of the distillate with i cc. of redistilled dimethylaniline, transfer
to a stout tightly stoppered flask, and keep on a bath at 70-80
292 ANALYSIS OF ALCOHOLIC BEVERAGES
for 3 hours, shaking occasionally. Make distinctly alkaline with
NaOH solution and distil off the excess of dimethylaniline, stop-
ping the distillation when 25 cc. has passed over.
Acidify the residue in the flask with acetic acid, shake, and
test a few cc. by adding 4 or 5 drops of a \% suspension of
PbO2. If methyl alcohol is present, there occurs a blue colora-
tion, which is increased by boiling. Ethyl alcohol thus treated
yields a blue coloration which changes immediately to green, later
to yellow, and becomes colorless when boiled.
68. Rlche and Bardy Method Official
The following method depends on the formation of methyl-
aniline violet:
Place 10 cc. of the sample, previously redistilled over K 2 COs
if necessary, in a small flask with 15 g. of I and 2 g. of red P.
Keep in ice KUO for 10-15 niinutes or until action has ceased.
Distil on a water bath into about 30 cc. of H^O, the methyl and
ethyl iodides formed. Wash with dilute alkali to eliminate free
I. Separate the heavy, oily liquid that settles and transfer to a
flask containing 5 cc. of aniline. If the action is too violent,
place the flask in cold H^O; if too slow, stimulate by gently
warming the flask. After an hour boil the product with H2O,
cool, and add about 20 cc. of 15% NaOH solution; when the
bases rise to the top as an oily layer, fill the flask up to the neck
with H2O and draw them off with a pipet. Oxidize i cc. of the
oily liquid by adding 10 g. of a mixture of 100 parts of clean
sand, 2 of NaCl, and 3 of Cu(NOa)2; mix thoroughly; transfer
to a glass tube; and heat to 90 for 8 10 hours. Exhaust the
product with warm alcohol, filter, and dilute to 100 cc. with
alcohol. If the sample is free from methyl alcohol, the liquid
has a red tint, but in the presence of \% of methyl alcohol it
has a distinct violet shade; with 2.5% the shade is very distinct
and still more so with 5%. To detect more minute quantities
of methyl alcohol, dilute 5 cc. of the colored liquid to 100 cc.
with H2O and dilute 5 cc. of this again to 400 cc. Heat the
liquid thus obtained in a porcelain dish and immerse in it a frag-
WATER-INSOLUBLE COLOR TENTATIVE 293
ment of white merino (free from S) for 30 minutes. If the
alcohol is pure, the wool will remain white, but if methyl alcohol
is present the fiber will become violet, the depth of tint giving
a fairly approximate indication of the proportion of methyl
alcohol.
69. Immersion Refractometer Method Official
Determine by the immersion refractometer at 20 the refrac-
tion of the distillate obtained in the determination of alcohol,
if, on reference to the table under A6, the refraction shows the
percentage of alcohol agreeing with that obtained from the spe-
cific gravity, it may be assumed that no methyl alcohol is present.
If, however, there is an appreciable quantity of methyl alcohol,
the low refractometer reading will at once indicate the fact. If
the absence from the solution of refractive substances other than
HaO and the alcohols is assured, this difference in refraction is
conclusive of the presence of methyl alcohol.
The addition of methyl alcohol to ethyl alcohol decreases the
refraction in direct proportion to the quantity present; hence
the quantitative calculation is made readily by interpolation in
the table under 72 of the figures for pure ethyl and methyl alcohol
of the same alcoholic strength as the sample being used.
Example. The distillate has a specific gravity of 0.97080,
corresponding to 18.38% alcohol by weight, and has a refraction
of 35.8 at 20 by the immersion refractometer; by interpolation
in the refractometer table the readings of ethyl and methyl al-
cohol corresponding to 18.38% alcohol are 47.3 and 25.4,
respectively, the difference being 21.9; 47.3 35-8=11.5;
(11.5-^21.9)100=52.5, showing that 52.5% of the total al-
cohol present is methyl alcohol.
70. COLORING MATTERS TENTATIVE
See under 51.
71. WATER-INSOLUBLE COLOR TENTATIVE
Evaporate 50 cc. of the sample just to dryness on a steam
bath. Take up with approximately 15 cc. of cold H 2 O, filter, and
294 ANALYSIS OF ALCOHOLIC BEVERAGES
72. TABLE Ai.
SCALE READINGS ON ZEISS IMMERSION REFRACTOMETER AT 20, CORRESPONDING TO
EACH PER CENT BY WEIGHT OF METHYL AND ETHYL ALCOHOLS
Per
Scale Read-
Per
Scale Read-
Per
Scale Read-
Per
Scale Read-
cent
ings
cent
ings
cent
ings
cent
ings
alco-
hol
by
weight
Methyl
alco-
hol
Ethyl
alco-
hol
alco-
hol
by
weight
Methyl
alco-
hol
Ethyl
alco-
hol
alco-
hol
by
weight
Methyl
alco-
hol
Ethyl
alco-
hol
alco-
hol
by
weight
Methyl
alco-
hol
Ethyl
alco-
hol
14-5
J 4-5
*5
29.7
60. i
50
39-8
90-3
75
29.7
IOI.O
i
14.8
16.0
26
30.3
61.9
51
39-7
91.1
76
29.0
IOI.O
i
J 5-4
17.6
^7
30-9
63.7
52
39-6
91.8
77
28.3
100.9
3
16.0
19.1
28
31-6
65.5
53
39- 6
92.4
78
27.6
100.9
4
16.6
20,7
29
32.2
67.2
54
39-5
93-
79
26.8
100.8
5
17.2
22.3
3
3*.8
69.0
55
39-4
93- 6
80
26.0
100.7
6
17.8
24.1
3i
33-5
70.4
56
39-*
94.1
81
25.1
100.6
7
18.4
25.9
32
34-1
71.7
57
39-o
94-7
82
24-3
100.5
8
19.0
27.8
33
34-7
73-i
58
38.6
95.2
83
23.6
100.4
9
19.6
29.6
34
35-*
74-4
59
38.3
95-7
84
22.8
100.3
10
20.2
31-4
35
35-8
75-8
60
37-9
96.2
85
21.8
100. 1
ii
20.8
33-2
36
36.3
76.9
61
37-5
96.7
86
20.8
99.8
12
21. 4
35-o
37
36.8
78.0
62
37-o
97-1
87
19.7
99-5
13
22.0
36.9
38
37-3
79.1
63
36.5
97-5
88
18.6
99.2
H
22.6
38.7
39
37-7
80.2
64
36.0
98.0
89
17-3
98.9
15
23.2
40-5
40
38.1
81-3
65
35-5
98.3
90
16.1
98.6
16
2 3-9
42.5
41
38.4
82.3
66
35-o
98.7
9 1
14.9
98-3
17
24-5
44-5
42
38.8
83-3
67
34-5
99.1
92
'3-7
97.8
18
25.2
46.5
43
39-*
84.2
68
34-0
99-4
93
12.4
97.2
19
25.8
48.5
44
39-3
85.2
69
33-5
99-7
94
II.
96.4
20
26.5
50-5
45
39-4
86.2
70
33-0
100.
95
9.6
95-7
21
27.1
52.4
46
39-5
87.0
7 1
3 2 -3
ICO. 2
96
8.2
94-9
22
27.8
54-3
47
39-6
87.8
72
31-7
IOO.4
97
6.7
94.0
2 3
28.4
56.3
48
39-7
88.7
73
3 1 -*
ico. 6
98
5- 1
93-0
24
29.1
58.2
49
39-8
89.5
74
30-4
100.8
99
3-5
92.0
100
2.0
91.0
wash until the filtrate amounts to nearly 25 cc. To this filtrate
add 25 cc. of absolute alcohol, or 26.3 cc. of 95% alcohol, and
make up to 50 cc. with H^O. Mix thoroughly and compare in
DETERMINATION 295
a colorimeter with the original material. Calculate from these
readings the percentage of color insoluble in H^O.
73. COLORS INSOLUBLE IN AMYL ALCOHOL TENTATIVE
Evaporate 50 cc. of the sample just to dryness on a steam
bath. Dissolve the residue in HkO and 95% alcohol and make
to a volume of 50 cc., using a total volume of 26.3 cc. of 95%
alcohol. Place 25 cc. of this solution in a separatory funnel and
add 20 cc. of freshly shaken Marsh reagent (100 cc. of pure
amyl alcohol, 3 cc. of sirupy H 3 PO 4 , and 3 cc. of H 2 O), shaking
lightly so as not to form an emulsion. Allow the layers to sepa-
rate and repeat this shaking and standing twice. After the layers
have separated completely draw off the lower or aqueous layer,
which contains the caramel, into a 25 cc. cylinder and make up to
volume with alcohol, 50% by volume. Compare this solution in a
colorimeter with the untreated 25 cc. Calculate from this reading
the percentage of color insoluble in amyl alcohol.
74. CARAMEL TENTATIVE
Add 10 cc. of paraldehyde to 5 cc. of the sample in a test
tube and shake. Add absolute alcohol, a few drops at a time,
shaking after each addition until the mixture becomes clear.
Allow to stand. Turbidity after 10 minutes is an indication of
caramel.
MARSH TEST FOR ARTIFICIAL COLORS TENTATIVE
(Caramel and Some Coal Tar Dyes)
75. REAGENT
Marsh Reagent. Prepare as directed under 73.
76. DETERMINATION
Place 10 cc. of the sample in a 20 cc. test tube, add sufficient
Marsh reagent to nearly fill the tube, and shake several times.
Allow the layers to separate; if the lower layer is colored, it is
296 ANALYSIS OF ALCOHOLIC BEVERAGES
an indication that the sample has been colored with caramel or a
coal tar dye.
In the absence of any color, test 10 cc, of the sample in the
same manner, using sufficient fusel oil, amyl alcohol or pentasol
to nearly fill the tube, and shake several times. A deeply colored
lower layer is an indication of a coal tar dye ; its identity should
be confirmed by using the methods under 51.
DETECTION OF METHANOL IN ALCOHOLIC BEVERAGES
77. REAGENT
(a) Potassium permanganate solution. Dissolve 3 g. of
KMnO4 in 15 cc. of 85% HsPOi and make up to 100 cc. with
H 2 O.
(b) Oxalic acid solution. Dissolve 5 g. of oxalic acid in
100 cc. of H2SO4 (i + i).
(c) Schiff's reagent. Dissolve 0.2 g. of Kahlbaum rosaniline
hydrochloride in 120 cc. of hot H^O, cool, add 2 g. of anhydrous
Na2SOs dissolved in 20 cc. of H2O, and 2 cc. of HC1, make up
to 200 cc., and store in well-filled glass-stoppered amber bottles.
78. DETERMINATION
Dilute the alcoholic beverage to 5% total alcohol by volume.
Transfer 5 cc. of this solution to a 6-inch test tube; add 2 cc.
of the KMnO4 solution; and let stand 10 minutes. Remove
the excess of KMnO4 by the addition of 2 cc. of the oxalic acid
solution. As soon as the KMnO4 is decolorized add 5 cc. of
Schiff's reagent. Mix thoroughly and let stand 10 minutes. If
HCHO is present, the characteristic reddish purple color is
produced.
Run blanks on pure ethyl alcohol and on ethyl alcohol con-
taining about \% of methanol.
CORDIALS AND LIQUEURS
297
CORDIALS AND LIQUEURS
No special methods for the examination of liqueurs and cor-
dials have been included in the Official and Tentative Methods of
Analysis of the Association of Official Agricultural Chemists.
The reader will find that the methods described above are gen-
erally applicable to this purpose. The following are suggested as
providing most of the determinations which will be required:
Paragraph
Physical Examination. i
Specific Gravity 3
Alcohol 4
Glycerol 9, 5, or 6
Total Solids 11
Sugars 14-^4
Non-sugar Solids 13
Ash 25
Ash-extract Ratio 26
Alkalinity of Water-
soluble Ash 27
Alkalinity of Water-
insoluble Ash 28
Total Acids 35
Paragraph
Volatile Acids 36, or 37
Fixed Acids 38
Total Tartaric Acid. . . 39
Tannin and Coloring
Matter 41
Gum and Dextrin 47
Coloring Matters and
Preservatives 51
Esters 59
Aldehydes 60
Furfural 61, 62
Fusel Oil 63, 64
Methyl Alcohol 67-69
Detection of Methanol. 77-78
ANALYTICAL REFERENCE TABLES
Aa-A?
TABLE Ai. DENSITIES OF SOLUTIONS OF CANE SUGAR AT 20 C.
Per cent
sugar
Tenths of Per Cent
Per cent
sugar
o
I
2
3
4
o
0.998234
0.998622
O.999OIO
0.999398
0.999786
i
I.OO2I2O
I.O025O9
1.002897
1.003286
1.003675
i
a
I.0060IS
I . 006405
1.006796
1.007188
1.007580
2
3
1.009934
I.OI0327
I.OIO72I
i. 011115
1.011510
3
4
I.OI388I
I.OI4277
I.OI4673
1.015070
1.015467
4
5
I.OI7854
I.OI8253
I.OI8652
1.019052
1.019451
5
6
I.02I855
I.O22257
1.022659
1.023061
1.023463
6
7
1.025885
1.026289
I.O26694
1.027099
1.027504
7
8
1.029942
1.030349
1.030757
1.031165
I.03I573
8
9
I.O34O29
1.034439
1.034850
1.035260
1.035671
9
10
1.038143
1.038556
1.038970
1.039383
1-039797
10
II
1.042288
1.042704
I.043I2I
1.043537
1.043954
ii
12
1.046462
I.04688I
I . 047300
1.047720
1.048140
12
13
1.050665
I.05I087
I.O5I5IO
I.05I933
1.052356
13
14
I.0549OO
1.055325
I.05575I
1.056176
1.056602
14
IS
I.059I65
1-059593
I.060O22
1.060451
1.060880
IS
16
1.063460
1.063892
1.064324
1.064756
1.065188
16
i?
1.067789
1.068223
1.068658
1.069093
1.069529
17
18
I.072I47
1.072585
1.073023
1.073461
1.073900
18
19
1.076537
1.076978
I.0774I9
1.077860
1.078302
i9
20
1.080959
1.081403
1.081848
1.082292
1.082737
20
21
1.085414
1.085861
1.086309
1.086757
1.087205
21
22
1.089900
1.090351
1.090802
1.091253
1.091704
22
23
1.094420
1.094874
1.095328
1.095782
i .096236
23
24
I.09897I
1.099428
1.099886
I . 100344
I . 100802
24
25
I- 103557
i .104017
I . 104478
I . 104938
i . 105400
25
26
I.I08I75
i . 108639
I.I09I03
i . 109568
1.110033
26
27
I.II2828
I.H3295
1.113763
1.114229
1.114697
27
28
I.H75I2
1.117982
I.II8453
1.118923
i. i 19395
28
29
I.I2223I
1.122705
I.I23I79
1.123653
1.124128
29
30
1.126984
1.127461
I.I27939
1.128417
1.128896
30
31
I.I3I773
1.132254
I.I32735
i. 133216
i . 133698
3*
32
I.I36596
1.137080
I.I37565
I . 138049
i . 138534
32
33
I.I4I453
1.141941
1.142429
r . 142916
I.I43405
33
34
I.I46345
1.146836
I.I47328
I . 147820
1.148313
34
35
I.I5I275
I.I5I770
I.I52265
1.152760
I.I53256
35
36
1.156238
1.156736
I.I57235
I. 157733
I.I58233
36
37
I.l6l236
1.161738
I.l62240
1.162742
1 . 163245
37
38
I . 166269
1.166775
1.167281
1.167786
I . 168293
38
39
I.I7I340
1.171849
I.I72359
i . 172869
1. 173379
39
40
I.I76447
1.176960
I-I77473
I.I77987
1.178501
40
41
I.l8l592
1.182108
1.182625
1.183142
I . 183660
4i
42
I.I86773
1.187293
1.187814
1.188335
1.188856
42
43
I.I9I993
1.192517
I . I9304I
I.I93565
i . 194090
43
44
I.I97247
I-I97775
I . 198303
1.198832
i . 199360
44
45
I . 202540
i . 20307 i
I . 203603
1.204136
I . 204668
45
46
1.207870
i . 208405
I . 208940
1.209477
1.210013
46
47
1.213238
i. 213777
I.2I43I7
1.214856
i. 2 i 5395
47
48
1.218643
1.219185
I.2I9729
i . 220272
1.220815
48
49
1.224086
1.224632
I.225I80
1.225727
1.226274
49
298
ANALYTICAL REFERENCE TABLES 299
TABLE As. DENSITIES OF SOLUTIONS OF CANE SUGAR AT 20 C. Continued
Per cent
sugar
Tenths of Per Cent
Per cent
sugar
5
6
7
8
9
o
.000174
.000563
.000952
.001342
.001731
o
i
. 004064
.004453
. 004844
.005234
.005624
i
2
.007972
.008363
.008755
.009148
.009541
2
3
.011904
.012298
.012694
.013089
.013485
3
4
.015864
.016261
.016659
.017058
.017456
4
5
.019851
.020251
.020651
.021053
.021454
5
6
.023867
.024270
.024673
.025077
.025481
6
7
.027910
.028316
.028722
.029128
.029535
7
8
.031982
.032391
.032800
.033209
.033619
8
9
.036082
.036494
.036906
.037318
.037730
9
10
.040212
.040626
.041041
.041456
.041872
10
ii
.044370
.044788
.045206
.045625
.046043
ii
12
048559
.048980
.049401
.049822
.050243
12
13
.052778
.053202
.053626
. 054050
.054475
13
14
.057029
057455
.057882
.058310
.058737
14
15
.061308
.061738
.062168
.062598
.063029
15
16
.065621
.066054
.066487
.066921
067355
16
17
.069964
. 070400
.070836
.071273
.071710
17
18
074338
.074777
.075217
075657
.076097
18
19
078744
.079187
.079629
.080072
.080515
19
20
.083182
.083628
.084074
.084520
.084967
20
21
.087652
.088101
.088550
.089000
.089450
21
22
.092155
.092607
.093060
.093513
.093966
22
23
.096691
.097147
.097603
.098058
.098514
23
24
.101259
.101718
.102177
.102637
. 103097
24
25
. 105862
. 106324
. 106786
.107248
.107711
25
26
.110497
. i 10963
.111429
.111895
.112361
26
27
. 115166
.115635
.116104
.116572
.117042
27
28
.119867
.120339
.120812
.121284
.121757
28
29
.124603
.125079
.125555
.126030
.126507
29
30
.129374
129853
. 130332
.130812
.131292
30
31
.134180
. 134663
.135146
.135628
.136112
31
32
. 139020
. 139506
139993
. 140479
. 140966
32
33
143894
.144384
.144874
145363
.145854
33
34
. 148805
. 149298
.149792
.150286
.150780
34
35
.153752
.154249
.154746
155242
.155740
35
36
.158733
-159233
159733
. 160233
. 160734
36
37
. 163748
.164252
.164756
.165259
.165764
37
38
.168800
. 169307
. 169815
.170322
.170831
38
39
. 173889
. 174400
.1749"
.175423
175935
39
40
.179014
.179527
. 180044
.180560
.181076
40
41
.184178
. 184696
.185215
185734
.186253
41
42
.189379
. 189901
.190423
. 190946
.191469
42
43
.194616
195141
.195667
.196193
.196720
43
44
. 199890
. 200420
. 200950
.201480
.202010
44
45
46
.205200
.210549
.205733
.211086
. 206266
.211623
. 206801
.212162
207335
.212700
a
47
.215936
.216476
.217017
.217559
.218101
47
48
.221360
.221904
.222449
.222995
.223540
48
49
.226823
.227371
.227919
.228469
.229018
49
300 ANALYSIS OF ALCOHOLIC BEVERAGES
TABLE Aa. DENSITIES OF SOLUTIONS or CANE SUGAR AT 20 C. Continued
Per cent
sugar
Tenths of Per Cent
Per cent
sugar
o
i
2
3
4
1 SO
1.229567
1.230117
. 230668
1.231219
1.231770
50
Si
i . 235085
i . 235639
.236194
i . 236748
237303
5i
52
i . 240641
1.241198
.241757
1.242315
. 242873
52
53
1.246234
i . 246795
247358
i . 247920
. 248482
53
54
1.251866
1.252431
.252997
1.253563
.254129
54
55
1-257535
i . 258104
.258674
i . 259244
.259815
55
56
1.263243
1.263816
. 264390
i . 264963
.265537
56
57
i . 268989
1.269565
270143
1.270720
.271299
57
58
1.274774
1.275354
.275936
1.276517
.277098
58
59
1.280595
1.281179
.281764
1.282349
.282935
59
60
i . 286456
i . 287044
.287633
1.288222
.288811
60
61
1.292354
1.292946
. 293539
1.294131
.294725
61
62
1.298291
1.298886
. 299483
1.300079
.300677
62
63
1.304267
1.304867
.305467
1.306068
. 306669
63
64
1.310282
1.310885
.3H489
1.312093
.312699
64
65
1.316334
1.316941
.317549
I.3i8i57
.318766
65
66
1.322425
1.323036
.323648
1.324259
.324872
66
67
1.328554
1.329170
.329785
1.330401
.331017
67
68
1-334722
1.335342
.335961
1-336581
337200
68
69
1.340928
i.34i55i
.342174
1.342798
343421
69
70
1.347174
i.3478oi
.348427
1.349055
.349682
70
71
I.353456
1-354087
.354717
1-355349
.355980
7i
72
1.359778
1.360413
.361047
1.361682
.362317
72
73
1.366139
1.366777
.367415
1.368054
.368693
73
74
1.372536
I.373I78
.373820
1.374463
375105
74
75
1.378971
i.3796i7
.380262
1.380909
.381555
75
76
1.385446
i . 386096
.386745
1-387396
.388045
76
77
1.391956
1.392610
.393263
I.3939I7
394571
77
78
1-398505
1.399162
.399819
1.400477
.401134
78
79
1.405091
1-405752
.406412
1.407074
407735
79
80
1.411715
1.412380
.413044
1.413709
.414374
80
81
1.418374
1.419043
.419711
i . 420380
.421049
81
82
1.425072
1.425744
.426416
1.427089
.427761
82
83
1.431807
1.432483
.433158
1.433835
-4345"
83
84
1-438579
1.439259
.439938
1.440619
441299
84
85
1.445388
1.446071
.446754
1.447438
.448121
85
86
1.452232
1.452919
.453605
1.454292
.454980
86
87
1.459114
1.459805
.460495
1.461186
.461877
87
88
1.466032
1.466726
.467420
1.468115
.468810
88
89
1.472986
1.473684
.474381
1.475080
475779
89
*
90
I.479976
1.480677
.481378
1.482080
.482782
90
9i
1.487002
1.487707
.488411
1.489117
.489823
9i
92
1.494063
I-49477I
495479
1.496188
.496897
92
93
1.501158
1.501870
.502582
1.503293
. 504006
93
94
1.508289
1.509004
.509720
1-510435
.5i"5i
94
95
I.5I5455
1.516174
.516893
1.517612
.518332
95
96
1.522656
1-523378
.524100
1.524823
.525546
96
97
1.529891
1.530616
.531342
1.532068
532794
97
98
1.537161
1.537889
.538618
1-539347
.540076
98
99
1.544462
I.545I94
.545926
1.546659
547392
99
100
1.551800
IOO
ANALYTICAL REFERENCE TABLES 301
TABLE Ai. DENSITIES OF SOLUTIONS OF CANE SUGAR AT 20 C. Continued
Per cent
sugar
Tenths of Per Cent
Per cent
sugar
5
6
7
8
9
50
1.232322
1.232874
i . 233426
1-233979
1-234532
50
5i
i - 237859
1.238414
1.238970
1.239527
i . 240084
5i
52
i . 243433
i 243992
1-244552
1-245113
i 245673
52
53
i . 249046
i . 249609
1.250172
1-250737
1.251301
53
54
i . 254697
1.255264
1.255831
i . 256400
1.256967
54
55
i . 260385
i . 260955
1.261527
1.262099
1.262671
55
56
1.266112
i . 266686
1.267261
1.267837
1.268413
56
57
1.271877
1-272455
i 273035
1.273614
1.274194
57
58
1.277680
1.278262
i . 278844
1.279428
1.280011
58
59
1.283521
r . 284107
i . 284694
1.285281
1.285869 .
59
60
i . 289401
1.289991
i . 290581
1.291172
1.291763
60
61
1.295318
1.295911
i . 296506
1.297100
i . 297696
61
62
1.301274
1.301871
1.302470
i . 303068
1.303668
62
63
1.307271
1.307872
1.308475
1.309077
i . 309680
63
64
1.313304
1-313909
I.3H5I5
1.315121
1.315728
64
65
I.3I9374
I.3I9983
1.320593
1.321203
1.321814
65
66
1.325484
1.326097
1.326711
1-327325
1.327940
66
6?
1.331633
1.332250
1.332868
1.333485
1.334103
67
68
1.337821
1.338441
1.339063
1.339684
1.340306
68
69
1.344046
1.344671
1-345296
1-345922
1.346547
69
70
1.350311
1.350939
I.35I568
I.352I97
1.352827
70
71
i .356612
1.357245
1.357877
1-358511
I-359I44
7i
72
1-362953
1.363590
1.364226
i . 364864
1.365501
72
73
1.369333
1.369973
1.370613
I.37I2S4
1.371894
73
74
1-375749
1-376392
1-377036
1.377680
1-378326
74
75
1.382203
1.382851
1.383499
1.384148
1-384796
75
76
1.388696
1.389347
I.389999
1.390651
1-391303
76
77
1.395226
1.39588!
1-396536
1-397192
1-397848
77
78
I.40I793
1.402452
1.403111
1.403771
i . 404430
78
79
i . 408398
1.409061
1.409723
1.410387
1.411051
79
80
1.415040
1.415706
1-416373
1.417039
1.417707
80
81
1.421719
1.422390
1.423059
1.423730
1.424400
81
82
1.428435
1.429109
1.429782
1.430457
1.431131
82
83
I.435I88
1.435866
1.436543
1.437222
1-437900
83
84
1.441980
1.442661
1.443342
1.444024
1.444705
84
85
1.448806
1.449491
I.450I75
1.450860
I.45IS45
fs
86
1.455668
1.456357
1.457045
1-457735
1.458424
86"
87
1.462568
1.463260
1.463953
i . 464645
1.465338
87
88
1.469504
i . 470200
1.470896
I.47I592
1.472289
88
89
1.476477
1.477176
1.477876
1.478575
1.479275
89
90
1.483484
1.484187
1.484890
1.485593
1.486297
90
9i
1.490528
1.491234
1.491941
1.492647
1-493355
9i
92
I.4976o6
1.498316
1.499026
1.499736
i . 500447
92
93
1.504719
1.505432
1.506146
I . 506859
1.507574
93
94
1.511868
1.512585
1.513302
1.514019
I.5I4737
94
95
96
1-519051
1.526269
1.519771
1.526993
1.520492
1.527717
1.521212
1.528441
I-52I934
1.529166
95
96
97
I-53352I
1.534248
1.534976
i - 535704
1-536432
9
98
I . 540806
I.54I536
1.542267
1.542998
1-543730
98
99
1.548127
1.548861
1-549595
1.550329
1.551064
99
100
100
302 ANALYSIS OF ALCOHOLIC BEVERAGES
I
(x
o
(x
o
o
CJ
o
X
o
Q
to
*
u ,
o
CO
55
(U
^
H
Cfl ~ M
J^
O oo vo ^ d O oo vo
r^i^-oooXOt-^M ci
OOO VO <<* M ON f- VOCOM ON r^ Vo CO M ON t^
vo vo VO r-OO OOON O w C* d CO ^ vovo VO t-
vo vo vo vovo vovo VO NO vO VO VO \O VO VO vo VO
. -, O Os
CNO s s
S S S S S
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s s s s s
10VO t^OO O\ OHttO* 10*O VO 00 ON O M N fO "<t IOO t^OO O\ O M M f> <
OkOkOkOkOk OOO OO O O O O O M M M M M HHHHH f* ft ft N ft
HHHHH ft ft tt r* ft <S tt <N <S <S NNNNN C1 n (1 ft N
* O ONO
DvS vov
VOVOVOVOVO vovovovovo vovovovovo
' ~~ i 1-1 O ONOO f--vo vo ^f co c< H-< O
vo vo vo vo Tt"
ONOO r-vo vo
co co co co c~
HHONr^VoCOMONr-Voc* O 00 VO <* C* OOOVO^C^ O OO VO CO HH ON f- vo CO fi
co co Tf vovo r- r^-oo ONO MMCJCO^^O vovo r--oo ONONO'-'C^ c<co^ vovo
OOOOO 6 O 6 O M M M M M i-I M M - M M I-II-HC<C<C< c<c<cir<c<
S.VQ \J fVj
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ro * 10 VO 1SOO Ok O H
1O 1O 1O 1O 1O 1O 1O 1O 1O V)
i w O Q O C
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vo vo ^j- co i-" '
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ONOO r^VO VO Tj- TJ- CO C< HH
HI O ^\oo r^ vo vo Tf ro <"
cococ4csc< csctctc*.
0000000000 OOOOOOOOOO 0000000000 0000000000 OOC_ .. _ ..
ONONONONO\ ONONONONON ONONONONON ONONONONON ONC^ONONON O\ONONONON
66666 66666 66666 66666 66666 6 6 6 6 6
vo c* O oo \O
0ovp "<he<Ooovo
O\0\O MCSCOCO^-
vo vo vovo NO vo NO vo VO vo VO VO vo vo vo NO t""^ r-* t^ r^- t^* t^
V\ S Ovts, VN
OvV Os ON CD S }
10 vo t>-oo a o H
^ vo' vd >d NO
t-OO Ok O H f) fO ^ 1OVO l>00 Ok
t^ t* t* 00 00 00 00 00 00 00 00 00 00
0\ Ok Ok 0\ (
vocoor--*^ c< ONr^^c< or-~voco>- ONT
oo r^vo <$ co c< O ONOO t^ vo ^ co M M ONO<
OOOOO OOONONON ONONONONONOOOOOOOOOO ooooooDor--r-<^i^-r--r^
ON ON ON ON ON ON ONOO oooo oooooooooo oooooooooo oooooocooo oooooooooo
ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON
ododo 66666 66666 00666 o' o o o o o o o o o
Qoovo^c* OoovocO"-* ONI^-VOCO*-" ONt^vocot-i ONt^'tfc^OoovO'^'CHO
O O M C* CO ^* 't 1 vovO t^ t^OOONO 1 " 1 wcico^t'vo vovo r--OOON ONO^c^co
oodoo ododo dod'-'^ MMMW^ ^ ^ M M M MM<SC<C^
OQ VQ ^f. (Vj Q OQ VQ \j* (\j Q (^ Vr^ <V\ s, ON tx, vr^ <V\ S Os tx, V^ cy^ s O\ ts^ Vr^ (Vj
Q K, <NJ <v^ ^j \J W^NO ts. OQ OQ Qy O "N *N C\j <Nrj >^ Vr^ VyO Ix^O Os Os O **i C\j f
ddo'dd ddddd dddss sssss sssss s <v <vi <M' <<
o M (s m Tt IONO i>oo Ok o M
ododo ddddd MM
10 vo t-oo a o H
O ^ O vo O vo O vo O vo O ^ O vO M vo * I s *- d t^ cooo ^f ON *o O vO d f^- co
O oo r-- vo TJ- c< HI ONOO vO vo co d O ON t--vo ifcot- Ooor^-voTi- coi-iOooi^.
Q ON ON ON ON ON ONOO oooo oooooooor- r-r^t^-r^r^- f^vo vOvovo vovovOvovo
QONONONON ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON
OOsONOsON ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON
Ddo'dd dddo'd ddddd ddo'dd ddddd odd do
ANALYTICAL REFERENCE TABLES
303
v> <M o oo vo 'fr c< O oo vo *f c O oo vo -J-MONr^^coMONr^oco
oo ON O -< c< co ^ ^t- *o vo r^oo oo ON O t-i M c< co ^ **> ^vO f- oo
r^- r-oo oooo oooooooooo OOOOOOQOOO o\ ON o\ o\ ON o\ ON 6\6\ o\ a\
fc&SSS
co co co co co c^clclc^cl dc^c
r-- r-- r t^- r^ r^ r^- r~~ r~^ r~~ i r^ r
ONONONONON ONONONONON ONONONONON
ONONONONON ON
ooooo ooooo ooooo ooooo ooooo o
CO M ON t^ vo d O
ONO O^c^corj-
}- <S O
-c*
CO VO CO M ON
-
O >h <>> s O\
Os O K? CNJ Pg
SSSS
Vrj Vrs Vrs V^ V
1
* 00 00 00 00 00 OOOOOOOOOO ON O)
00 00 r- r-XO VOVOVOU-.XO
ONOO r^-\O ^o rj- o c*
ONONONONON ONONON
t^ r^'r^- r^-t-~ r^-r^r^- -
ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON O\ONONONON
66666 06006 00666 66666 60006 66666 06006
C^ co ^T vovo vo t^oo ON ON O M ol
300000O OOOOOOOOOO 00 00 00 00 ON ONONONONON ONONO\O\ON ONONQOO
. OsN.
N.OO OO Os O S^ <M r*>
oO
OsOsOs OsOsOsOsOs OsOsOsOsO O O O O O
O H N fO * 10VO h-OOO> OH^cO^t
o o o o d o o o o o M M M M H
h-OO O O M
ON O
5 vo r-oo ON (
ONVOMVOd oo ThOvOc* ONVOMOO rf- O^Dco ONVO c ON vo c< oo -o cS ONVO co O r~- -^ M
vo ^t- co M O oo r->vo j- CO M O ON r-VO vococ^OONOOVOvorj-c< MQOO t^-vo vo co C< M
ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON ONONONO<
ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON ONONONONON ONONONO>
ooooo ooooo ooooo o o 666 ooooo 66666 60660
II
ss
og
11
o
I
B .
s
I
a .2
304 ANALYSIS OF ALCOHOLIC BEVERAGES
ON r-> vo d O oovo -"td O oovo co M ON r^^co-i ON
r-oo ON O M MC^CO-^-*^ vrvo t^-oo oo ON O M d d
vo VO vO vo vO vO vo VO VO
u-0'
(S
N ts.O O O
mo roo ON o M n eo ^ ioso i>oo o\ o H
O\O\O\dtO\ OOOOO OOOOO M M M
t-oo o\ o M N ro ^t
N Ci f< n N N N N
ftfe
00 I^VO v rj- CO d O 00 f-*VO vo
Vo vo vo vo vo vr> vo vo vo rj- ^ -^ rf-
t^VO ^o
HH O ONC
co cod
5 ^f ^ ^ co^> CO co CO co co
ON ON ON ON ON ON ON ON ON ON ON ON ON ON ON ONONONONON ONONONONON ONONONONON
66666 66666 66666 66666 66666 66666
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i-C< Q
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ANALYTICAL REFERENCE TABLES
305
VO H-clQoo so -rj-t-i ON r-- vncot-i ON r- *t <S O oo so "1- d O oo so co
r->oo ON o o M <s co co <$ ^'"O r-* r-oo ON o -< * c* co <* ^ *^NO r^
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306 ANALYSIS OF ALCOHOLIC BEVERAGES
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5/5 M'OOOO 66666 66666 66666 66666 66666
ANALYTICAL REFERENCE TABLES
.307
vO'^t'C4Ooovoco>-ONr-~voco-<oovo*t'r<Ooovoco>-'ONr i ~-voco .o'S
vo r^oo ONON O^dc^fO <* *^vo vor^ooONOOMMcoco-'t'VoNO -
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3 o8 ANALYSIS OF ALCOHOLIC BEVERAGES
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3io ANALYSIS OF ALCOHOLIC BEVERAGES
J8.I
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ANALYTICAL REFERENCE TABLES 311
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312 ANALYSIS OF ALCOHOLIC BEVERAGES
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ANALYTICAL REFERENCE TABLES
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314 ANALYSIS OF ALCOHOLIC BEVERAGES
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ANALYTICAL REFERENCE TABLES 315
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316 ANALYSIS OF ALCOHOLIC BEVERAGES
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ANALYTICAL REFERENCE TABLES
317
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318 ANALYSIS OF ALCOHOLIC BEVERAGES
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^^
^
00 O
H
co m
l> <<fr
M oo in
O H CO
in R oo o N
o t* in N o
Tt- in t^ a M
00 vo CO M O\
< o oo o>
M" co in 2- a
a oo t*
v^oT
o
***
^^^ ^^
.****
555
^t- O tx
4 4
tx
tx CX
o
(V) Cg
^^
ii$
^c^^c^^
^;U
s;;*^
^^
*^
H t-
c< CO
CO
in
S#
S'S
Tt- H 00
co in vo
^ M oo in co
oo o H co in
&^?s a
S S, 8 1
cO H 00 vo 't
^ vo t^ O\ H
S8.SS
Sin
^
oo oo
00
oo oo
O
% % %
O
O O M M M
^ ^t ^t t *fr
M M M (H
Tf Tj- ^- ^t 1 ^-
555
fO 't
* *
5
tx
c^
O **")
3&
<vj tx fvj tx ^
CX O cvj ") ^O
OQ co op rj- C5\
Xi OQ CX H C\|
vo O O S Xi
>txi tx ex o
c\j co vo Xi oo
VQ Cn
N Cr
%^
5
>s>
s>
s>^
5^^
coc^SJ,
<\j fr) ff) f^ tv-)
^ <% % 55 ^
Sc^Sco'
$$$$$
^^^
^
^
H VO
3
^s
vo
fr- 00
N oo in
M CO
M 00 * H 00
in vo oo o M
co in oo o
S S5K t2 a
$*% 5vS (
a Z n
$^
*?i
?n
?n*
00 00
ro $ 3
C\ 0\
^ ^ 5-
M M H M H
^ 5- 5- ^ S
^55
5 5
*>
O f
Tf
<000
<N
"frVO 00
o *<o oo
O N "t<> 00
O N TflO 00
O N * VO 00
^
to oo
t* 1-
t-
22
rt- ^
s s
1CIC 1C 5C 1C
^.^^.^^
KSKRR
oo oo oo oo oo
S S S
t^ t"
,8
320 ANALYSIS OF ALCOHOLIC BEVERAGES
TABLE Ay. MUNSON AND WALKER'S TABLE * FOR CALCULATING DEXTROSE, INVERT
SUGAR ALONE, INVERT SUGAR IN THE PRESENCE OF SUCROSE (0.4 GRAM AND 2 GRAMS
TOTAL SUGAR), LACTOSE, LACTOSE AND SUCROSE (a MIXTURES), AND MALTOSE
(CRYSTA LLIZED)
(Expressed in milligrams)
Cuprous oxide (Cu20)
'$
O
1
a
Dextrose (d-glucose)
S
9
tO
8
) 1
Invert Sugar and
Sucrose
Lactose
Lactose and
Sucrose
Maltose
Cuprous oxide (Cu2O) |
3
o
+J
B ui
&>>
*"
o
3
o
cfl M
I!
c*
q
w
+
1
u
%
II
w
<+
1
JJ2
M
w
-f
3
w
u
10
12
14
16
18
20
22
24
26
28
30
32
34
36
38
40
42
44
46
48
50
52
54
56
58
60
62
64
66
68
70
72
74
76
78
80
82
84
86
88
8. 9
10.7
12.4
14.2
16.0
17.8
19-5
21.3
23.1
24-9
26.6
28.4
30.2
32.0
33-8
35-5
37-3
39-1
40.9
42.6
44.4
46.2
48.0
49-7
51.5
53-3
55.1
56.8
58.6
60.4
62.2
64.0
65.7
67.5
69.3
71.1
72.8
74.6
76.4
78.2
4-o
4-9
5-7
6.6
7-5
8-3
9-2
IO.O
10.9
ii. 8
12.6
13-5
14-3
15-2
16.1
16.9
17-8
18.7
19.6
20.4
21.3
22 . 2
23.0
23-9
2 4 .8
25-6
26.5
27.4
28.3
29-2
30-0
30-9
31-8
32.7
33-6
34-4
35-3
36.2
37-1
38.0
4-5
5-4
6-3
7.2
8.1
8.9
9.8
10.7
ii. 6
12.5
13-4
14-3
15-2
16.1
16.9
17-8
!8. 7
19.6
20.5
21.4
22.3
23.2
24.1
25-0
25-9
26.8
27.7
28.6
29-5
30.4
31-3
32.3
33-2
34-1
35-0
35-9
36.8
37-7
38.6
39-5
1.6
2-5
3-4
4-3
5.2
6.1
7-0
7-9
8.8
9-7
10.7
n. 6
12.5
13-4
14-3
15-2
16.1
17.0
17-9
18.8
19-7
20.7
21 .6
22.5
23-4
24-3
25.2
26. 2
27.1
28.0
28.9
29-8
30.8
31-7
32.6
33-5
34-5
35.4
36.3
37-2
6.3
7-5
8.8
IO.O
11.3
12.5
13-8
15-0
16.3
17.6
18.8
20. I
21.4
22.8
24.2
25-5
29.6
28.3
29.6
31.0
32.3
33-7
35-1
36.4
37-8
39-2
40.5
41-9
43-3
44-7
46.0
47-4
48.8
50.1
51-5
52-9
54-2
55-6
57-0
58.4
6.1
7-3
8.5
9-7
10.9
12. I
13-3
14-5
15-8
17-0
18.2
19-4
20.7
22. O
23-3
24-7
26.O
27-3
28.6
30.0
31-3
32.6
34-0
35-3
36.6
37-9
39-3
40.6
41-9
43-3
44.6
45-9
47-3
48.6
49-9
51-3
52.6
53.9
55-3
56.6
6.2
7-9
9-5
II. 2
12-9
14-6
16.2
17-9
19.6
21.2
22.9
24.6
26.2
27.9
29.6
31-3
32.9
34-6
36.3
37-9
39-6
41-3
42.9
44-6
46.3
48.0
49.6
5L3
53-0
54.6
56.3
58.0
59-6
61.3
63.0
64.6
66.3
68.0
69.7
71.3
10
12
I i
16
18
20
22
24
26
28
30
32
34
36
38
40
42
44
46
48
50
52
54
56
58
60
62
64
66
68
70
72
74
76
78
80
82
84
86
88
4-3
5-2
6.1
7.0
7-9
8.8
9-7
10.7
ii. 6
12.5
13-4
14-3
15-2
16.2
17.1
18.0
18.9
19.8
20.8
21.7
22.6
23-5
24-5
25-4
26.3
27-3
28.2
29.1
30.0
3LO
40.7
4L9
43.1
44.2
45.4
46.6
47-8
49.0
50.1
51.3
52.5
*U. S. Bur. Standards Circ. 44, p. 321. The columns headed "Lactose" and "Lactose and Su-
crose" are taken from "Methods of Sugar Analysis and Allied Determinations" by Arthur Given.
ANALYTICAL REFERENCE TABLES
TABLE Ay. MUNSON AND WALKER'S TABLE. (Continued)
(Expressed in milligrams)
321
q
x-x
Invert Sugar and
Sucrose
Lactose
Lactose and
Sucrose
Maltose
f
o
8
q
9,
U
T3
o
"bo
t4
3
-g
W
w
a;
73
g
U
2,
ri
o
+
3?
t
1
uprous
1
o
M
tJ
1
a n
jtf ctf
IJf
w) ^
if
So w
1
a,- o
1^
Is
q
1
CO
1
U
U
Q
Q
(-H
6
u
M
H
u
u
90
79.9
38.9
40.4
38.2
31-9
59-7
57-9
53-7
73.0
90
92
81.7
39-8
41.4
39-i
32-8
61.1
59-3
54-9
74.7
92
94
83.5
40.6
42.3
40.0
33-8
62.5
60.6
56.0
76.3
94
96
85.3
41.5
43-2
41.0
34-7
63.8
61.9
57-2
78.0
96
98
87.1
42.4
44.1
41-9
35-6
65.2
63.3
58.4
79.7
98
IOO
88.8
43-3
45-0
42.8
36.6
66.6
64-6
59-6
81.3
IOO
102
90.6
44-2
46.0
43-8
37-5
68.0
66.0
60.8
83.0
IO2
104
92.4
45.1
46.9
44-7
38.5
69-3
67.3
62.0
84.7
104
106
94-2
46.0
47.8
45-6
39-4
70.7
68.6
63.2
86.3
106
108
95-9
46.9
48.7
46.6
40.3
72.1
70.0
64.4
88.0
108
no
97-7
47-8
49-6
47-5
41-3
73-5
71-3
65.6
89.7
IIO
112
99-5
48.7
50.6
48.4
42.2
74-8
72.6
66.7
91-3
112
114
101 .3
49-6
51-5
49.4
43-2
76.2
74-0
67.9
93-0
114
116
103.0
50.5
52.4
50-3
44.1
77-6
75-3
69.1
94-7
116
118
104.8
5L4
53-3
51-2
45-0
79.0
76.7
70.3
96-4
118
120
106.6
52.3
54-3
52.2
46.0
80.3
78.0
71-5
98.0
1 20
122
108.4
53-2
55-2
53-1
46.9
81.7
79-3
72.7
99-7
122
124
IIO.I
54-1
56.1
54-1
47-9
83.1
80.7
73-9
101.4
124
126
in .9
55-0
57-0
55-0
48.8
84-5
82.0
75-1
103.0
126
128
113-7
55-9
58.0
55-9
49-8
85.8
83-4
76.3
104.7
128
130
II5-5
56.8
58.9
56.9
50.7
87.2
84.7
77-5
106.4
130
132
II7-3
57-7
59-8
57-8
51-7
88.6
86.0
78.7
108.0
132
134
119.0
58.6
60.8
58.8
52.6
90.0
87.4
79-7
109.7
134
136
120.8
59-5
61.7
59-7
53-6
91.3
88.7
81.1
111.4
136
138
122.6
60.4
62.6
60.7
54-5
92-7
90.1
82.3
113.0
138
140
124.4
61.3
63.6
61.6
55-5
94-1
91.4
83.5
114.7
140
142
I26.I
62.2
64-5
62.6
56.4
95-5
92.8
84.7
116.4
142
144
127.9
63.1
65-4
63.5
57-4
96.8
94-1
85-9
118.0
144
146
129.7
64.0
66.4
64-5
58-3
98.2
95-4
87.1
II9-7
146
148
I3I.5
65.0
67.3
65-4
59-3
99-6
96.8
88.3
121.4
148
ISO
133.2
65-9
68.3
66.4
60.2
IOI.O
98.1
89.5
123.0
150
152
135-0
66.8
69.2
67.3
61.2
102.3
99-5
90.8
124.7
152
154
136.8
67.7
70.1
68.3
62.1
103.7
100.8
92.0
126.4
154
156
138.6
68.6
71.1
69.2
63-1
105.1
IO2.2
93-2
128.0
156
158
140.3
69.5
72.0
70.2
64.1
106.5
103.5
94-4
129.7
158
1 60
I42.I
70.4
73.0
71.2
65.0
107.9
104.8
95-6
131-4
160
162
143.9
7L4
73-9
72.1
66.0
109.2
106.2
96.8
133-0
162
164
145.7
72.3
74-9
73.1
66.9
1 10. 6
107.5
98.0
134.7
164
166
147-5
73-2
75.8
74.0
67.9
112.
108.9
99-2
136.4
1 66
168
149-2
74-1
76.8
75-0
68.9
113.4
1 10. 2
100.4
138.0
168
322 ANALYSIS OF ALCOHOLIC BEVERAGES
TABLE Ay. MUNSON AND WALKER'S TABLE. (Continued)
(Expressed in milligrams)
1
^
Invert Sugar and
Sucrose
Lactose
Lactose and
Sucrose
Maltose
1
CJ
1
q
O
CJ
<u
"3
^
'to
M
3
^
CU
ffi
-8
cj
cu
w
'K
o
CJ
v ~ x
?
M
_o
_
en
-2
,_
o
(A
$
2
CO
+J
is
IS
i
Jji
CU u
q
l/J
&
a
U
) f
Z ?
w
t> m
t; N
W
&
3
o
CU
3
CJ
CJ
Q
1 1
o
*
CJ
H
H
CJ
CJ
170
151.0
75-1
77-7
76.0
69.8
114.8
in. 6
IOI.6
139-7
170
172
152.8
76.0
78.7
76.9
70.8
116.1
112.9
102.8
141.4
172
174
154.6
76.9
79-6
77.9
71-7
H7.5
114-3
104.1
143.0
174
176
156.3
77-8
80.6
78.8
72.7
118.9
115.6
105.3
144.7
176
178
158.1
78.8
81.5
79-8
73-7
120.3
117.0
106.5
146.4
178
1 80
159-9
79-7
82.5
80.8
74-6
121. 6
118.3
107.7
148.0
180
182
161.7
80.6
83-4
81.7
75-6
123.1
119.7
108.9
149-7
182
184
163.4
81.5
84.4
82.7
76.6
124-3
121.
IIO.I
151-4
184
1 86
165.2
82.5
85.3
83.7
77.6
125.8
122.4
in. 3
153-0
186
1 88
167.0
83-4
86.3
84.6
78.5
127.2
123.7
112.5
154-7
1 88
190
168.8
84-3
87.2
85.6
79-5
128.5
I25-I
113.8
156.4
190
192
170.5
85.3
88.2
86.6
80.5
129.9
126.4
115.0
158.0
192
194
172.3
86.2
89.2
87.6
81.4
131-3
127.8
116.2
159-7
194
196
174.1
87.1
90.1
88.5
82.4
132.7
129.2
117.4
161.4
196
198
175-9
88.1
9I-I
89.5
83.4
134-1
130.5
118.6
163.0
198
200
177-7
89.0
92.0
90-5
84.4
135-4
I3I.9
119.8
164.7
200
202
179-4
89.9
93-o
85.3
136.8
133-2
121.
166.4
202
2O4
181.2
90.9
94-0
92-4
86.3
138.2
134.6
122.3
168.0
2O4
206
183.0
91.8
94-9
93-4
87.3
139-6
135-9
123.5
169.7
206
208
184.8
92.8
95-9
94-4
88.3
141.0
137.3
124.7
171.4
208
210
186.5
93-7
96.9
95-4
89.2
142.3
138.6
I26.O
173-0
2IO
212
188.3
94.6
97.8
96.3
90.2
143-7
140.0
127.2
174-7
212
214
190.1
95-6
98.8
97.3
91-2
145. i
I4I.4
128.4
176.4
214
216
191.9
96.5
99.8
98.3
92.2
146.5
142.7
129.6
178.0
216
218
193-6
97-5
100.8
99-3
93-2
M7-9
I44.I
130.9
179-7
218
2 2O
195-4
98.4
101.7
100.3
94-2
149-3
145-4
I32.I
181.4
22O
222
197.2
99-4
102 7
101.2
95- *
150.7
146.8
133.3
183.0
222
224
199.0
100.3
103.7
IO2.2
96.1
152.0
I48.I
134-5
184.7
224
226
200.7
101.3
104.6
103.2
97-1
153-4
149.5
135.8
186.4
226
228
202.5
IO2.2
105.6
104.2
98.1
154-8
150.8
137.0
188.0
228
230
204.3
103.2
106.6
105.2
99.1
156.2
152.2
138.2
189-7
230
232
206.1
I04.I
107.6
106.2
100. 1
157-6
153-6
139-4
I9L3
232
234
207.9
I05-I
108.6
107.2
IOI.I
159-0
154-9
140.7
193-0
234
236
209.6
106.0
109.5
108.2
IO2.I
160.3
156.3
I4I.9
194.7
2 3 6
238
211.4
107.0
110.5
109.2
IO3.I
161.7
157-6
143.2
196-3
238
24O
213.2
108.0
in. 5
IIO.I
104.0
163.1
159-0
144.4
198.0
240
242
215-0
108.9
112.5
in. i
105.0
164.5
160.3
145.6
199-7
2 4 2
244
216.7
109.9
II3-5
112. I
106.0
165.9
161.7
146.9
201.3
244
2 4 6
218.5
no. 8
114.5
II3.I
107.0
167.3
163.1
I48.I
203.0
246
248
220.3
in. 8
115.4
II4.I
108.0
168.7
164.4
149-3
204.7
248
ANALYTICAL REFERENCE TABLES
TABLE A7 MUNSON AND WALKER'S TABLE. (Co ntinued)
(Expressed in milligrams)
323
q
Invert Sugar and
Sucrose
Lactose
Lactose and
Sucrose
Maltose
O
If
tn
3
B
1
q
q
u
'H
^
1
8
3
3
+
g
ffl
V
rs
'H
U
^
=?
*
2
. &
^
o
to
tn
to
S i*
to u,
6
iT 2
q
en
1
a
Q,
t-t
H
1
8>!
cj a'
1
3 |
Jg
3 "
W
I
P,
3
o
53
>
J2J H
3
U
U
P
P
t 1
d
u
H
H
u
U
250
222.1
112. 8
116.4
115-1
109.0
170.1
165.8
150.6
206.3
250
252
223.8
II3-7
117.4
116.1
IIO.O
171.5
167.2
I5I-8
208.0
252
254
225.6
114.7
118.4
117.1
III.O
172.8
168.5
I53-I
209.7
254
256
227-4
II5-7
119.4
118.1
112. O
174.2
169.9
154.3
211.3
256
2 5 8
229.2
116.6
120.4
119.1
II3.0
175-6
155-5
213.0
258
260
231.0
117.6
121.4
1 20. i
II4.O
177.0
172.6
156.8
214.7
260
262
232.7
118.6
122.4
121. I
II5.0
178.4
174.0
158.0
216.3
262
264
234-5
II9-5
123.4
122. I
116.0
179-8
175-3
159-3
218.0
264
266
236.3
120.5
124.4
I23-I
117.0
181.2
176.7
160.5
219.7
266
268
238.1
121.5
125.4
I24.I
118.0
182.6
I78.I
161.8
221.3
268
270
239.8
122.5
126.4
I25.I
119.0
184.0
179-4
163.0
223.0
270
272
241.6
123.4
127.4
126.2
120.0
185.3
180.8
164.3
224.6
272
274
243-4
124.4
128.4
127.2
121. I
186.7
182.2
165-5
226.3
274
2 7 6
245.2
125.4
129.4
128.2
122. I
188.1
183-5
166.8
228.0
276
278
246.9
126.4
130.4
129.2
123-1
189.5
184.9
168.0
229.6
278
280
248.7
127.3
131.4
130.2
I24.I
190.9
186.3
169.3
231.3
280
282
250.5
128.3
132.4
I3T .2
I25-I
i9 2 -3
187.6
170.5
233.0
282
284
252.3
129.3
133.4
132.2
I26.I
193-7
189.0
171.8
234.6
284
286
254-0
130.3
134-4
133 2
I27.I
I95-I
190.4
173.0
236.3
286
288
255-8
131.3
135-4
134-3
I28.I
196.5
174-3
238.0
288
290
257.6
132.3
136.4
135-3
129.2
197-8
I93-I
175-5
239 . 6
290
292
259-4
133-2
137-4
136.3
130.2
199-2
194-4
176.8
241.3
292
294
26l.2
134.2
138.4
137-3
I3I-2
200. 6
195-8
178.1
242.9
294
296
262.9
135-2
139-4
138.3
132.2
202. o
197.2
179-3
244.6
296
298
264.7
136.2
140.5
139-4
133-2
203.4
198.6
180.6
246.3
298
300
266.5
137-2
I4L5
140.4
134-2
204.8
199-9
181.8
247-9
300
302
268.3
138.2
142.5
I4I.4
135-3
206.2
201.3
183-1
249-6
302
304
27O.O
139-2
143-5
142.4
136.3
207.6
202.7
184.4
251-3
304
306
271.8
140.2
144-5
143-4
137-3
209.0
204.0
185.6
252.9
306
308
273.6
141.2
145.5
144-5
138.3
210.4
205.4
186.9
254.6
308
310
275.4
142.2
146.6
145-5
139-4
211. 8
206.8
188.1
256.3
310
312
277.1
143-2
147.6
146.5
140.4
213-2
208.1
189.4
257-9
312
314
278.9
144.2
148.6
147-6
141.4
214,6
209,5
190.7
259-6
314
316
280.7
145.2
149.6
148.6
142.4
216.0
210.9
191.9
26l .2
3i6
318
282.5
146.2
150.7
149.6
143-5
217.3
212.2
193-2
262.9
3l8
320
284.2
147-2
I5I.7
150.7
144-5
218.7
213.6
194-4
264.6
320
322
286.0
148.2
152.7
I5L7
145-5
220. i
215-5
195-7
266.2
322
324
287.8
149.2
153-7
152.7
146.6
221/5
2l6.4
197.0
267.9
324
326
289.6
150.2
154.8
153-8
147.6
222.9
217.7
198.2
269.6
326
328
291.4
151.2
155.8
154.8
148.6
224.3
2I9.I
199.5
271.2
328
324 ANALYSIS OF ALCOHOLIC BEVERAGES
TABLE Ay. MUNSON AND WALKER'S TABLE. (Continued)
(Expressed in milligrams)
Invert Sugar and
Sucrose
Lactose
Lactose and
Sucrose
Vlaltose
Q
s
w
U
U
TJ
13
13
W
W
1
U
3
8)
+
4)
Cfl
+
g
tfl
10
M
d **
q
2
of o
q
!
o
t->
H 5)
1 5>
&
2 OT
2
u
6
I
M
o
as
u
*
H
1-5 H
H
u
a
u
330
293.1
152.2
156.8
155.8
149-7
225-7
220.5
200.8
272.9
330
332
294.9
153.2
157.9
156.9
150.7
227.1
221.8
2O2.O
274.6
332
334
296.7
154-2
158.9
157.9
I5I-7
228.5
223.2
203-3
276.2
334
336
298.5
155-2
159-9
159.0
152.8
229.9
224.6
204.6
277-9
336
338
300.2
156.3
161.0
160.0
153-8
231.3
226.0
205.9
279-5
338
340
302.0
157.3
162.0
161.0
154.8
232.7
227.4
207.1
281.2
340
342
303.8
158.3
163.1
162,1
155-9
234.1
228.7
208.4
282.9
342
344
305.6
159-3
164.1
163.1
156.9
235-5
230.1
209.7
284.5
344
346
307.3
160.3
165.1
164.2
158.0
236.9
231.5
211.
286.2
346
348
309.1
161.4
166.2
165.2
159.0
238.3
232.9
212.2
287.9
348
350
310.9
162.4
167.2
166.3
160.1
239-7
234-3
213-5
289.5
350
352
312.7
163-4
168.3
167-3
161.1
241.1
235.6
214.8
291.2
352
354
314-4
164.4
169.3
168.4
162.2
242.5
237-0
216.1
292.8
354
356
316.2
165.4
170.4
169.4
163.2
243.9
238.4
217-3
294-5
356
358
318.0
166.5
171.4
170.5
164.3
245-3
239-8
218.6
296.2
358
360
319.8
167-5
172.5
I7L5
165.3
246.7
241.2
219.9
297-8
360
362
321.6
168.5
173.5
172.6
166.4
248.1
242.5
221.2
299-5
362
364
323.3
169.6
174.6
173.7
167.4
249-5
243-9
222.5
301.2
364
366
325-1
170.6
175.6
174-7
168.5
250.9
245-3
223.7
302.8
366
368
326.9
171.6
176.7
175-8
169-5
252-3
246.7
225.0
304-5
368
370
328.7
172.7
177.7
176.8
170.6
253-7
248.1
226.3
306.1
370
372
330.4
173.7
178.8
177-9
171.6
255-1
249-5
227.6
307-8
372
374
332.2
174-7
179-8
179.0
172.7
256.5
250.9
228.9
309.5
374
376
334-0
175-8
180.9
180.0
173-7
257.9
252.2
230.2
311.1
376
378
335-8
176.8
182.0
181.1
174.8
259-3
253-6
23L5
312.8
378
380
337-5
177.9
183.0
182.1
175.9
260.7
255-0
232.8
3M.5
380
382
339-3
178.9
184.1
183.2
176.9
262.1
256.4
234-1
316.1
382
384
34I-I
180.0
185.2
184-3
178.0
263.5
257-8
235-4
317.8
384
386
342-9
181.0
186.2
185.4
I79-I
264.9
259-2
236.6
319.4
386
388
344-6
182.0
187-3
186.4
180.1
266.5
260.5
237-9
321.1
388
390
346.4
183.1
188.4
187.5
181.2
267.7
261.9
239.2
322.8
390
392
348.2
184.1
189.4
188.6
182.3
269.1
263.3
240.5
324.4
392
394
350-0
185.2
190.5
189.7
183.3
270.5
264.7
241.8
326.1
394
396
351.8
186.2
191.6
190.7
184.4
271.9
266.1
243.1
327.7
396
398
353-5
187.3
192.7
191-8
185-5
273-3
267.5
244.4
398
400
355-3
188.4
193.7
192.9
186.5
274.7
268.9
245-7
331- 1
400
402
357-1
189.4
194-8
194.0
187.6
276.1
270.3
247.0
332-7
402
404
358.9
190.5
195-9
i95-o
188.7
277.5
271.7
248.3
334-4
404
406
360.6
I9I.5
197.0
196.1
189.8
278.9
273-0
249-6
336.0
406
408
362.4
192.6
198.1
197.2
190.8
280.3
274-4
251.0
337-7
408
ANALYTICAL REFERENCE TABLES
TABLE Ay. MUNSON AND WALKER'S TABLE. (Continued)
(Expressed in milligrams)
325
f
1
Invert Sugar and
Sucrose
Lactose
Lactose and
Sucrose
Maltose
1
Si
q
q
U
r$
^
Tjb
1
P-H
W
0)
8
U
^
>
3
-1-
i-l
g>
"t
1
M
p
&
I
2
I s
J2 M
H 0$
1
II
f i
q
3
*
Q<
a
o
8
1
!*!
1^ E?
bO w
%
1 *
ctf H
e*
a
U
U
Q
M
6
N
U
H
H
U
U
410
364-2
193.7
I99.I
198.3
I9I.9
281.7
275-8
252.3
339.4
410
412
366.0
194.7
2OO.2
199-4
193-0
283.2
277.2
253-6
341.0
412
414
367.7
195-8
2OI-3
200.5
I94.I
284.6
278.6
254-9
342.7
414
416
369-5
196.8
202.4
2OI.6
195.2
286.0
28O.O
256.2
344.4
416
418
371.3
197-9
203.5
2O2.6
196.2
287.4
281.4
257.5
346.0
418
420
373-1
199-0
2O4.6
203.7
197-3
288.8
282.8
258.8
347.7
420
422
374-8
200. i
205-7
204.8
198.4
290.2
284.2
260.1
349-3
422
424
376.6
2OI.I
206.7
205-9
199-5
291.6
285.6
26l.4
351-0
424
426
378.4
2O2.2
207.8
2O7.O
2OO.6
293.0
287.0
262.7
352.7
426
428
380.2
203-3
208.9
208. I
201.7
294.4
288.4
264.O
354-3
428
430
382.0
204.4
2IO.O
209.2
202.7
295.8
289.8
265.4
356.0
430
432
383.7
205-5
211. I
210.3
203 . 8
297.2
291.2
266.6
357-6
432
434
385 - 5
206.5
212.3
2II.4
204.9
298.6
292.6
268.0
359-3
434
436
387.3
2O7.6
213-3
212.5
206.0
300.0
294.0
269.3
361.0
436
438
389-1
208.7
214.4
213.6
207.1
301.4
295.4
270.6
362.6
438
440
390-8
209.8
215-5
214.7
208.2
302.8
296.8
272.O
364-3
440
442
392-6
210.9
216.6
215-8
209.3
304-2
298.2
273-3
365-9
442
444
394-4
212.0
217.8
216.9
210.4
305.6
299.6
274.6
367.6
444
446
396-2
2I3.I
218.9
218.0
211.5
307.0
3OI.O
275-9
369-3
446
448
397-9
2I4.I
22O.O
219.1
212.6
308.4
302.4
277.2
370-9
448
450
399-7
215.2
221. 1
22O.2
213-7
309.9
303.8
278.6
372.6
450
452
401.5
2l6.3
222.2
221.4
214.8
3H.3
305.2
279-9
374-2
452
454
403-3
217.4
223.3
222.5
215-9
312.7
306.6
28l.2
375-9
454
456
405.1
218.5
224.4
223.6
217.0
314-1
308.0
282.5
377-6
456
458
406.8
219.6
225.5
224.7
218.1
315.5
309.4
283.9
379-2
458
460
408.6
22O.7
226.7
225.8
219.2
316.9
310.8
285.2
380.9
460
462
410.4
221.8
227.8
226.9
220.3
318.3
312.2
286.5
382.5
462
464
412.2
222.9
228.9
228.1
221.4
319.7
313.6
287.8
384.2
464
466
413.9
224.0
230.0
229.2
222.5
321.1
315.0
289.2
385.9
466
468
415.7
225.1
231.2
230.3
223.7
322.5
316.4
290.5
387.5
468
470
417.5
226.2
232.3
231.4
224.8
323-9
317.7
291.8
389-2
470
472
4I9-3
227.4
233-4
232.5
225.9
325.3
3I9.I
293.2
390-8
472
474
421.0
228.3
234.5
233-7
227.0
326.8
320.5
294-5
392-5
474
476
422.8
229.6
235-7
234-8
228.1
328.2
32L9
295-8
394-2
476
478
424.6
230.7
236.8
235-9
229.2
329.6
323.3
297.1
395-8
478
480
426.4
231.8
237-9
237-1
230.3
331-0
324.7
298.5
397-5
480
482
428.1
232.9
239-1
238.2
231.5
332.4
326.1
299.8
399-1
482
484
429.9
234-1
240.2
239-3
232.6
333.8
327.5
30I.I
400.8
484
486
431-7
235.2
241.4
240-5
233.7
335-2
328.9
302.5
402.4
486
488
433-5
236.3
242.5
241.6
234-8
336.6
330-3
303.8
404.1
488
490
435-3
237.4
243.6
242.7
236.0
338.0
331-7
305.1
405.8
490
CHAPTER XV
STATISTICS OF THE LIQUOR INDUSTRY
The importance of reliable and ample statistics to modern
business is now widely recognized and in the last two decades
the Federal Government and various trade associations have
placed a vast amount of data at the disposal of the corporation
executive.
While the Federal Government has compiled statistics of the
liquor production and trade for at least three decades, unfortu-
nately the prohibition era has interfered; so that such figures as
are available cannot present an accurate picture of the liquor
trade as we have known it to exist for the 1918 to 1932 period.
There are presented here a selection of statistical tables
taken mainly from government publications and compilations
obtained therefrom; which indicate with some accuracy the
trends in the United States production and consumption of wines
and liquors. The data are presented with a reservation that
their accuracy, at best, is qualitative.
Size of the industry. That the industry was formerly both
large and widespread is shown by the fact that in 1901 there
were 3,736 distilleries in operation, of which 1,258 used grain
and 2,478 used fruit as raw material.
By 1914 there were only 352 grain and 368 fruit distilleries
operating, or a total of 720. Since production increased during
this fourteen year period, we have evidence of merger into fewer
and larger units.
According to recent data (Dec., 1933) there are registered 6
grain, 2 molasses and 25 fruit distilleries. All but five of the fruit
distilleries are operating. In addition there are 43 industrial
alcohol plants operating. See Table 27 for complete data.
In 1907, and again in 1912, over $156,000,000 in taxes were
collected on withdrawals of distilled spirits. The Government
326
FOREIGN TRADE IN DISTILLED SPIRITS 327
collected $186,947,000 in 1917, $308,429,000 in 1918 and
$353,737,000 in 1919. Taxes on wine ranged from $2,307,000
in 1915 to $11,474,000 in 1919. See Table 28.
In 1901 there remained aging in bonded warehouses after
the annual withdrawals 154,438,407 gallons of distilled spirits.
By 1914 the bonded warehouses held, after annual withdrawals,
286,900,000 gallons; of which 278,108,000 were whiskey,
1,217,000 rum, 216,000 gin, 4,865,000 brandy and 2,495,000
alcohol. See Table 29. In 1913 the industry used 4,252,583
bushels of malt and 5,828,450 bushels of rye in addition to other
cereals. See Table 30.
Production of distilled spirits. Production of distilled spirits
exclusive of alcohol averaged 89,900,000 gallons from 1901 to
1914, reaching a maximum of 114,634,000 gallons in 1913.
Production of whiskey increased from 89,700,000 gallons in
1901 to an average of 99,400,000 for the three year period
1911 to 1913 inclusive.
Production of rum increased from 1,724,000 gallons in 1901
to 3,026,000 gallons in 1914.
Production of gin increased from 1,636,000 gallons in 1901
to 4,012,543 gallons in 1914.
Production of brandy increased from 4,047,000 gallons in
1901 to 7,307,800 gallons in 1914.
Production of alcohol in 1901 was 41,458,000 gallons and
81,101,000 gallons in 1915. Practically a 100 per cent increase
in 15 years. By 1926 it had more than doubled to 202,270,000
gallons. It jumped from 79,900,000 in 1922 to 122,400,000 in
1923. Prior to that time 10,000,000 gallons was the highest
jump, war years excepted. See Table 31 for more complete data.
Withdrawals of distilled spirits. Withdrawals of distilled
spirits exclusive of alcohol increased from 60,585,000 gallons in
1901 to 83,577,000 gallons in 1913 and to 93,210,000 in 1917,
a war year. They declined abruptly in 1920 to 6,394,000 and
reached a low of 1,000,000 gallons in 1932. See Table 32.
Foreign trade in distilled spirits. Exports of distilled spirits
averaged 1,400,000 gallons for the 15 year period 1901 to 1915
inclusive. , j ;.
328 STATISTICS OF THE LIQUOR INDUSTRY
Exports of rum held fairly level for the 8 year period 1910
to 1917 and averaged 1,250,000 gallons.
Exports of whiskey declined from 685,729 gallons in 1901
to 155,880 gallons in 1918. They spurted suddenly to 3,315,861
in 1920, preceding prohibition. See Table 33.
Germany, Mexico, the Philippine Islands, South America,
England, Central America, Canada and Bermuda have been our
best customers for whiskey. Following prohibition, Bahama
Islands, Bermuda, Canada, Cuba, England and Mexico all re-
ceived large shipments, most of which probably found its way
back to us via the bootleggers. See Table 34.
Imports of distilled liquors remained fairly level during the
period 1901 to 1918 and averaged 3,450,000 gallons a year.
Imports of whiskey remained fairly level during the period
1910 to 1917 and averaged 1,420,000 gallons per year.
Imports of brandy averaged 494,000 gallons for the period
1901 to 1917.
Imports of gin averaged 955,000 gallons for the period
1910 to 1916.
Imports of cordials averaged 472,000 gallons for the period
1912 to 1916. See Table 35.
Consumption of distilled spirits. Theoretically, the ap-
parent consumption of distilled spirits may be calculated as
follows. Withdrawals from bonded warehouses, plus imports,
minus exports should give the apparent consumption. Unfor-
tunately, in the last seven or eight years bootleggers succeeded
in diverting large amounts of industrial alcohol to alcoholic bev-
erages. Since this diversion was considered to amount to a
large volume, any estimate of consumption during prohibition
must include an allowance for industrial alcohol and must be arbi-
trary at best. By reference to Table 31 it will be observed
that there was a tremendous expansion in industrial alcohol pro-
duction for the period 1922 to 1932. However, in the period
1901 -to 1915 production increased 100 per cent so that large ex-
pansion in this industry is not unknown. On the other hand, in
the period 1905 to 1914 production averaged 71,570,000 gallons
and in the period 1919 to 1922, 90,350,000 gallons. Production
WINE CONSUMPTION 329
then increased rapidly, more than doubling (from 90,000,000 to
200,000,000) in the next four years, 1922 to 1926, and main-
tained a high rate thereafter.
If increased industrial consumption during 1922 to 1926 ac-
counted for one-half of the increased production then the remain-
ing half probably represents the amount diverted by bootleggers.
In other words, 25 per cent of any increase over the 1919 to
1922 average.
On this basis an estimate of consumption has been arrived
at for the period 1901 to 1932 and is shown in detail in Table
36. In period 1901 to 1919 consumption averaged 70,120,000
gallons. In period 1925 to 1932 it averaged 41,050,000 gallons
with a high of 52,292,000.
It is impossible to determine whether prohibition really did
cut consumption to this extent or whether too small credit has
been given to the bootleg industry. However, by another method
of the consumption it might be pointed out that in the 16 years
1901 to 1916 the gross increase of withdrawals was roughly 28
per cent. On this basis, if the normal increase for the next 16
years has been at the same rate then withdrawals in 1932 would
have amounted to 98,630,000 gallons so that consumption would
have been something slightly over 100,000,000 gallons allowing
for excess of imports over exports.
Wine consumption. Statistics on wine are divided into two
classifications, namely, still wines, and champagne and other
sparkling wines.
Production (total) of wines was fairly constant for the period
1912 to 1919 averaging 45,600,000 gallons and reaching a high
of 55,756,000 gallons in 1919. Thereafter it dropped sharply,
averaging 6,800,000 gallons for the period 1922 to 1932. See
Table 37.
Exports of wine for the period 1901 to 1915 averaged
786,000 gallons. From 1916 to 1920 exports increased from
1,133,000 gallons to 4,573,000 gallons. Thereafter there was a
sharp drop to 26,000 gallons in 1921 and in the period 1926
to 1932 exports were too negligible to record. See Table 38.
Imports of wine for the period 1901 to 1918 averaged
330 STATISTICS OF THE LIQUOR INDUSTRY
5,969,000 gallons of still wines; and 913,000 gallons of cham-
pagne and other sparkling wines. It is interesting to note that
the period 1903 to 1910 marked the largest consumption. Cham-
pagne imports then averaged well over 1,000,000 gallons an-
nually, and still wines also jumped to well over 7,000,000 gallons
a year and even to 9,500,000 in 1910. Following enactment of
prohibition there was a sharp drop to an average of 33,700 gal-
lons of still wines and champagnes for the period 1924 to 1931.
See Table 39.
By combining the data in Tables 37-39 apparent consump-
tion of wine is obtained. For the period 1912 to 1919 it aver-
aged 49> 2 33>ooo gallons.
Following prohibition it dropped to an average of 6,033,000
gallons for the period 1924 to 1932, with a high of 11,403,000
for the boom year 1929. See Table 40.
The liquor industry as a consumer of agricultural products.
The advocates for repeal of prohibition have made much of
the large outlet for farmers' crops which the liquor industry will
present. It is not within the scope of this book to consider the
crops and amounts consumed by the beer brewing industry.
Reference to Table 30 shows that in 1913 the distilled
liquor industry used 4,252,000 bushels of malt and 5,828,000
bushels of unmalted rye. In addition some portion of the corn
and molasses consumption of 23,800,000 bushels and 64,600,000
gallons respectively must also be allocated to the liquor industry
although larger proportions went into the manufacture of alcohol.
In 1925 the liquor industry used 96,170,000 pounds of raisins
and 682,000 pounds of rice besides other materials.
Another factor to be taken into consideration and which, so
far, has not had a great deal of publicity is the potential outlet
for fruit surpluses. For example, applejack from apples; cordials
and liqueurs from peaches, pears, oranges, apricots, plums, cher-
ries, prunes, herbs and seeds, etc.
The possible future of the industry can be visualized by refer-
ences to Table 41 which shows that in 1930 France produced
MO9, 933,000 gallons, Italy 551,737,000 gallons, Spain 481,-
585,000 and other countries similar large amounts of wine.
THE LIQUOR INDUSTRY
TABLE 27. DISTILLERIES REGISTERED AND OPERATED AND INDUSTRIAL-ALCOHOL PLANTS
OPERATED, FISCAL YEARS 1901 TO 1932, INCLUSIVE
Fiscal
year
Grain
Molasses *
Fruit
Indus-
trial
alcohol
plants
oper-
ated f
Total
oper-
ated*
Regis-
tered
Oper-
ated
Regis-
tered
Oper-
ated
Regis-
tered
Oper-
ated
1901
1902
1903
1904
1905
1906
1907
1908
1909
1910
1911
1912
*9 J 3
1914
1915
1916
1917
1918
1919
1920
1921
1922
'923
1924
1925
1926
1927
1928
1929
1930
I93i
1932
1,506
i,37*
W5
M3 1
896
912
878
799
690
633
588
575
528
475
438
338
301
154
i5
8
2
2
1,258
1,089
1,103
744
728
740
7 IO
579
4 66
444
432
417
398
35*
249
279
198
72
13
6
2
2
9
ii
'3
15
14
14
15
*5
X 7
18
18
19
23
25
*3
25
27
27
25
21
2 "
2
2
2
2
2
2
2
2
2
2
2
9
ii
12
'5
*3
13
'5
14
16
16
17
18
22
*3
23
25
25
27
23
21
2
2
2
2
2
2
2
2
2
2
2
2
2,515
1,869
i,378
i,453
1,108
1,215
919
667
840
470
504
401
469
380
386
337
297
192
38
21
32
3 1
3 1
23
24
^7
22
^5
32
25
20
^5
2,478
1,838
1,326
1,413
IP3 1
1,132
862
607
810
446
474
386
450
368
363
301
28 4
137
38
20
29
30
31
23
24
27
22
25
32
25
20
20
3,745
2,938
2,441
2,172
i,772
1,885
i,587
1,200
1,292
906
923
821
870
743
635
605
57
236
74
9i
102
102
98
95
97
93
86
82
86
84
75
7i
44
69
68
65
70
7i
64
62
55
52
5o
46
43
7
7
6
7
7
6
* Rum only manufactured since 1921.
t Industrial-alcohol plants use both molasses and grain in manufacture of alcohol.
332 STATISTICS OF THE LIQUOR INDUSTRY
TABLE 28. TAX COLLECTED ON DISTILLED SPIRITS, WINES AND FERMENTED LIQUORS,
FISCAL YEARS 1901 TO 1932, INCLUSIVE
Year
Distilled spirits
Wines
Fermented liquors
Total
iqoi
Jll6 % O27.q7q.c6
7C 669 907 6c
$ 69788721
^
iqO2
f * w,v- ^ yy / y j^
7I,q88,qO2.iq
iqi.I26,qiC.C2
.7
I qoi
1 1 1. QC 1.4.72. 1O
/ yy V 9y oy
47,547,856.08
~yo* yy j j
I7q. COI. 128.4.7
1004
o yy jOvr/ jy
135,810,015.42
4q.o8l,4C8.77
/.7Jj v *>O 'T/
l84.8qi,474.iq
iqoC
t7J OJT^J / /
* w *r> w i/O,^/T^ x
i86,iiq % o66.io
y j
IQ06
!4l > iq4 > OCC 12
Cc'64/8c8 c6
>O 'yj^'^ ^"o
IQQ.OIC qii.68
*yww
Ic6.1l6.QOI.8q
Co <67*8i8 18
yyy ojyy o v
2lC.qO4.72O.O7
iqo8
* 3 W >OO V >.7 .7
140,158,807.15
59,807,616.81
j,y v *t, / *^ > -' /
Iqq.q66,421.q6
AVfW
134,868,034.12
57,456,41 1 .42
yyyy v y^ ~o y
IQIO
l4.8.O2q,1II.C4-
60,572,288.54
208,601,600.08
IQII
^ v y y?O 7^
64, 167,777. 6c
*y* A
1912
i56',39M35-77
$52.00
T 1 ^O / ' / / / J
63,268,770.51
219,660,258.28
19*3
163,879,276.54
66.00
66,266,989.60
230,146,332.14
IQIA
i Co 008 177 11
67.08 1. C 1 2.4 C
226.I7q68q.76
1915
142,312,397.40
2,307,30! -97
/ ) tj ^j
7q 128 q4o72
* v j /yy y i
223,948,646.09
I9l6
156,050,909.55
2,631,529.98
88,771,103.99
247,453,543-5 2
1917
186,947,243.78
5,164,075.03
91,897,193.81
284,008,512.62
I9l8
308,429,318.77
9,124,368.56
126,285,857.65
443,839,544.98
1919
353,737,44-77
11,474,207.49
117,839,602.21
483,050,854.47
I92O
93,161,205.60
4,744,070.11
41,965,874.09
139,871,149.80
1921
80,281,612.55
2,316,452.46
25,363.82
82,623,428.83
1922
44,257,100.75
1,306,249.72
46,086.00
45, 6 9,43 6 -47
1923
28,822,015.50
1,531,991.38
4,078.75
30,358,085.63
1924
26,126,317.76
1,454,062.88
5,327.73
27,585,708.37
1925
24,307,331.65
1,595,488.63
1,954-44
25,904,774.72
1926
24,756,900.06
1,679,434.38
15,694,19
26,452,028.63
1927
20,399,065.88
795,602.83
883.25
21,195,551.96
1928
14,414,088.04
893,408.41
300.00
15,307,796.45
1929
12,484,078.53
292,549.93
IOO.OO
12,776,728.46
IDOO
II 4.CC 88l QQ
2iq,i8l.68
ii 60 c 267 67
I 11
10*201* C6q 41
O.7>O W O w
2284.qC.o6
10,432,064.49
I 12
g' ' ' g
XT7 J
8.701.061.27
>
'
,/ oyy o /
THE LIQUOR INDUSTRY
333
TABLE 29. SPIRITS REMAINING IN BONDED WAREHOUSES JUNE 30, 1901, TO 1932
BY KINDS
[Statement in tax gallons]
Year
Whiskey
Rum
Gin
Brandy
Alcohol
Aggregate
1901
150,652,832.5
679.302.7
268,105.7
1,705,269.7
1,132,897.1
154,438,407.7
1902
164,388,547.8
949,430.1
246,526.8
2,077,254.1
3,157,925.8
170,819,684.6
1903
183.930,488.3
1,229,162.2
172,118.6
2,757,382.8
3,019,009.0
191,108,160.9
1904
191,320,875.7
1,310,632.4
255,073-1
2,775,088.3
2,249,344.6
197,911,014.1
1905
210,780,752.6
,195,443.9
320,568.9
3,177,271.9
3,260,558.2
218,734,595-5
1906
223,737.332-0
,188,675.5
273,231.3
2,226,587.0
1,536,590.0
228,962,415.8
1907
242,319,516.7
,222,581.1
242,370.8
2,153,250.4
1,654,347.4
247,592,066.4
1908
231,940,083.4
,227,008.5
201,176.3
2,966,215.6
1,657,860.0
237,992,343.8
1909
226,096,519.0
,108,327.9
181,479.0
3,679,936.7
i,755,io8.i
232,821,370.7
1910
230,224,625.0
820,268.5
161,604.8
4,137,844.5
2,302,176.3
237,646,519.1
1911
246,203,020.4
983,387.6
214,794.0
4,519,762.1
1,878,144.6
253,799,io8.7
1912
260,074,282.8
984,953.3
190,278.3
5,001,083.6
2,536,317-4
268,786,915.4
1913
272,504,285.5
1,086,063.4
180,458.0
5,784,226.8
3,013,733-1
282,568,766.8
I9M
278,108,056.1
1,217,302.7
216,016.2
4,865,324-7
2,495,085.2
286,901,784.9
1915
249,714,721.4
1,218,392.7
234,965-4
6,143,372.3
2,500,261.8
259,811,713.6
1916
228,677,774.1
906,042.5
216,911.5
5,849,015-4
2,602,150.2
238,251,893.7
1917
189,675,854-7
966,644.5
533,065.0
4,244,404.8
3,657,118.4
199,257,087.4
1918
140,721,821.5
741,104.2
2,777,467.7
3,494,020.8
14,718,871.1
162,453,285.3
1919
63.942,931.5
460,709.6
1,551,101.8
1,260,344.9
6,403,408.2
73,618,496.0
1920
50,550,498.6
413,923.8
963,996.7
884,025.1
3,935,326.1
56,747,770.3
1921
3996i,943.8
399,419.1
885,912.9
641,558.1
8,643,577.4
50,532,411.3
1922
36,588,568.3
384,012.2
987,884.7
963,781.5
7,068,291.1
45,992,537.8
1923
33,151,029.0
366,244.2
878,597.2
1,269,206.5
7,364,040.9
43,029,117.8
1924
30,064,670.9
341,214.0
836,730.2
1,289,400.8
6,697,627.3
39,229,643.2
1925
26,840,953-5
327,379.1
8i9,599.3
1,229,141.7
9,641,420.9
38,852,494.5
1926
23,814,140.2
289,344-6
802,433.2
1,133,057.7
6,249,064.2
32,288,039.9
1927
20,904,071.2
252,329.5
8i9,443.7
1,029,598.0
9,263,241.6
32,268,684.0
1928
17,975,943-8
282,387.2
815,718.2
1,013,305.2
7,u3,533.3
27,200,887.7
1929
15,127,390.8
226,830.6
794,447.5
906,702.8
12,075,898.9
29,131,270.6
1930
14,786,971-9
171,409.8
799,587.6
864,141.1
10,375,534.0
26,997,644-4
i93i
15,179,327.9
188,648.2
781,191.8
971,828.5
16,346,160.8
33,467,157-2
1932
15,293,713.1
200,305.2
746,076.2
1,020,895.9
19,223,942.03
36,484,932.43
334 STATISTICS OF THE LIQUOR INDUSTRY
g
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cortc^vo ONOO >- Qvfi cooo coQ
rcoo ON^ covo rf-t^ONCS ^--^-t-< r^Tj-c cooo
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* T? i-T ? r? oo" OO^ O** T? >-T rp CO ^ cToo" t^ O^ ON ON CO ^ ON
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ONONONONONONONONONONONON
THE LIQUOR INDUSTRY
335
Tf-i^t osvo HI d co v" H co c
T3 o
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3 4
vo oo covo I"*- M d r^- Os ^- oo
cooo vo vooo^ d^ rp^ 4 ^
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r, 1
xf- d vo r^ ^ o vo co M oo TJ-
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r~^ T*- vo vo'rf OSOO vo T|- ^- O
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336 STATISTICS OF THE LIQUOR INDUSTRY
TABLE 31. DISTILLED SPIRITS PRODUCED DURING FISCAL YEARS 1901-1932
[Production shown in tax gallons]
Year
Whiskey
Rum
Gin
Brandy
Alcohol
Total
exclusive
of alcohol
1901
1902
1903
1904
1905
1906
1907
1908
1909
1910
1911
1912
I9'3
1914
IOI C
79,701,170
75,414,812
70,673,93*
60,606,978
71,083,421
70,633,074
86,552,027
54,502,027
70,152,174
82,463,894
100,647,155
98,209,574
99,615,828
88,698,797
A A CC2 4.8O
1,724,582
2,202,047
2,247,906
1,801,179
1,791,987
1,730,101
2,022,407
1,895,922
i>95 2 5 374
<W3>949
2,631,059
2,832,515
2,750,846
3,026,085
2 SAA ill
1,636,299
1,752,280
1,913,404
2,110,215
2,187,709
2,323,^89
2,947,687
2,756,752
2,483,743
2,985,435
3,345,37
3,577,86i
4,014,600
4,012,542
7,6'?6,28c
4,047,602
4,220,400
6,43 ,673
5, J 93>262
5,448,584
4,444P7i
6,138,304
6,899,822
6,440,857
7,656,433
7>953, I 3 I
9,321,823
8,252,874
7,307,897
8.C2I,OCI
41,458,547
49,254,261
66,940,959
6 9>793>578
72,747, 6 76
7o,979, 6 6o
77,051,166
67,835,037
58,862,463
68,534,247
68,778,809
75*630,032
78,972,108
78,874,219
81,101,063
89> I0 9, 6 53
83,589,539
81,265,914
69,7^,634
80,511,701
79,^0,555
97,661,049
66,054,523
81,029,248
95*3 59*7! i
I 4,57 6 ,7 I 5
"3,944,773
114,634,148
103,045,321
jyi j
1916
1917
1918
IOIO
59,240,671
57,651,834
17.383.5"
2,986,940
2,842,921
1,526,743
8IC/7Q4.
4,118,064
5,756,666
4,i78>538
4,159,35!
8,251,097
5,357*325
1,802,422
182,778,245
211,582,744
150,387,680
08,160,121
1 War
i y*y
IQ2O
ooj. 7Q{
QAA Ql6
1. 640, AA C
08.4.16.170
IQ2I
X J4/ W }
7C7 '2*74.
C4.7 CO*7
If 70 7Q2
8< 068 776
IQ22
/!>JO/4
or C 7QQ
JT-JjJ^/
864..'n2
1,077,061
70,006,101
IO21
J 1 jy/yy
8OC.122
1,417,461
122,402,849
J y-*j
I O24.
784.608
84.7.IO4.
IK,8o7,72C
I QIC
784. 086
C4.7.727
i66.i6c.<i7
x y z i
1926
804.. 706
641.068
202,271,670
102*7
8lO 4.4.Q
118,4.10
1 84., 121,016
1 y- i /
1028
QO.'KO
411, cic
169,149,904
iy^o
IQ2Q
1. 227.4. 11
1. 1 Q4.2Q2
200,832,051
xyxy
TQ'JO
I Qo8 QA*7
082 78l
4.I6.O4.1
1 01. 8 CO. 14,2
iyju
I O*J I
*>yy>y4/
o Aic 671
I TOO 077
82O.278
166.014.14.6
1 yj 1
IO7.2
^^Jij^ 1
I 711 O28
i > x- *j>y//
I .OQJ..777
6lO,786
146,010.012
i yj z
Source: "Statistics concerning intoxicating liquors," Bureau of Industrial Alcohol,
U. S. Treasury Department, Washington, D. C.
THE LIQUOR INDUSTRY
337
vo vo ON o vo r^-o ^t-o
vo co vn co ON ON O co
Kft *o i-i'vb d i-t vb Q vd O" < <?ONr^vndNO S o' S *-"vn > ^(xToo"^ ? T? o" 4 vo" -
P 00 hi vnvo ONt-i ON ON vn ON ON "fr F*^ ^ CT" ^ ^ . 2> V? ^ >5 ^ !> ^ ^ ^ * f~rS?
vo vn ^ T$- xj- vnvo vO vO " "" " " ~ ~
5
tn
D
ONH-idi-<vnt-H r^oooovo d ON ^ O O cooo
co Ji d d d oo oo i i O vo ON ON d ''t' ^J* O O vo i i r *-" TJ- ^- ON s vo ** d oo HH ON co
ON hj\ t~~- O O oo d cooo r O Ovoo TJ- ON ^t~vo vn ONOO oo co co O vo ^t" d vnvo ON O d
KJ) d ^J- O d co >" t^ HH co co d vnoo oo oo oo d O vo O vn - vn d ~ "~ ~" - - ~-
o < cT 4^ 4 r^ r-^ 4 vn* kTscToo' 4 -" r --~ - r - ~ r -" - ~ -" - * -" r
o
N
ONOO r|- ON vn ^vo ON d HH vnoo cocoOvO >-* O O vnO\ONCOdoooo d r^co "J-vp ON
WQ d r ^ ^ ON >-i H^ { co co vn d r*- cooo f~ d ON O vnvo oo >* o | - 4 CA ****'* ~ "
J~ O\ vn i-^ -f Tj- d^ -^00^ ^00^ t^ t-^ -^ CO C^^ i-^ vo vn co O\ ' ^ '
O VO O VO VO vO vn O ON ON ^t" r ^" I vnoo ON HH vo vn ON vn i-< co d (* "' co vn d HH oo
^5 NO r--oo vn r-oo COH o ^covncot^I^-r^O coOvo c< cor^-co vnoo d vo oo d co -"
O^vn-^r^r^-ONi-ro O\vn vnvo ONOO cooo HI ONOO d vo vo O ONOcToo oo oo^ocToo"
CO ^vO vO VO VO r-vo rhvnvnvnvnvnvnvnt^-d M d d M -
fi
^
co-" T^OVOOO ^ONt^r^ ONVO ^Mdi-tcovnH-tO'-'vnH-iH-idO covo ^ ON ^-vo
Q bJD ^ ooHHvo-i-dvovnr^.codvOdr*-doo ^-oo oo oo oo vn tl-oo vn d r^vo ^-co vp -" vo
~" 5 oo vo ^t* ^* c*> CO ON d co ^ co ^ vn o d O M ON d ON vnNO covo O vo vo O oo
5 t-ONHitncoH-Tt-r-ONHidooQ 1^^ *** *^ O^ 00 O vo d d d ' ' '
H X X j j ***. ,^t~L _i. iV r^ Xi o vX ^v r^oo vn d O ^
Ol
o 1
^ "> oo co r^oo vo l^- H vn ONVO ON l^vo ONVO oo oo oo co rt-vo - ONVO vO vo oo HH co co
00 oo d co d" r^ 6 M o\ O vd co d* oo* ON 4oo ' 6 6 oo oo O vn 4- 4vd ~ 4 d d M O
_.--* co t^ O -^- co ONOO d r^r-d Qvncod -^-d d H ONO vnvo oo i- vn d ^ r-oo HH o
O vn^o S e? H^VO^VO ON ON O^ 0\ ON d 5 ?- 5 ***O. ' ^ cod^n-tcoddHH
^ i-Tt-Ti-rcrdddddd'cocori-cofo
B
!*. ON r- ON ONVO ^ONdvO ONHHOO cod ^r- vnoo ONVO O oo ON O vO O\ O
-. e d* oo' ON ONVO' -I co -' -*' oo* 6 - 6 6 4 O vn ^ vn ONOO 4- ^ c< M ^ cooo d r^ d
H C co co ^ O -^ vnvo co vnoo ooQvnd fO-"CO-"CO IH ONvn r-oo r- d O ONOO <*
PH H^ocT *cTvnT?o*NO' % coo"r^-vn-4rf 4'vo" O^ *-T o^ >-T 0*00* co cT ^ O^ocT fC *" -^ -- "
PCO ON "T t^- O ONVO CO HH ON ON >H O vnvO "^ vn COVO d"-t MHIMMMHH
r^ r-oo oo ONOO ONVO ^ NO vo r- r-vo vnvovo co "
r*- co co covo r^oo o >-< r^oovo ^coo ON ONVO
*** {.. (-Ivnvncor^r- 4oo vo 4-O\O-< COON4-ON>-| O ^vndvO O\ -> cooo oo covo O d
2?P r--.oor-r--vnO covo O\oov5 'too O 4 co ON ONOO ~ - "
^ ^Q 1 ^^ ^ *! ^S *^ ^ ^ ^ ^t ^i ^^ ^ ^ ^ ^ ^
r^oo*oo* i-T T|- co co ONVO O d vn -d-vo ^hoo HH d d r^oo"vd
M ^J-MMCO-^-O ON-t ONOO vn rho -! vo ON d -^-00 HH INO _ . . _ _
i_i Q\ M vo c< vn r^ O vn d vo co d oo vo ^t" vn d ** HH M vo r~~~oo ONOO NO vn vn TJ- d ON
r^ T? vn vn vn <oo\ d^r^d^dvo^rTroO^ covo dVOONd"i-<HiH-iH-iN-ii-<M-ii-r
\n vn ^f rj- ^ -^f vn vnvo vo r- r- r- r-vo vo oo vnvo
? Q f^ "^ VT^^ r^op ON O M d co ^ vnvo r-oo ON O w d I co "t vnvp r^oq ON O
>^
338 STATISTICS OF THE LIQUOR INDUSTRY
TABLE 33. EXPORTS DISTILLED SPIRITS, 1901 TO 1932
In gallons
Year
Brandy
Rum
Whiskey B
Whiskey R
All other
Total
1901
1902
1903
1904
1905
1906
1907
1908
1909
IQIO
i5>323
24,077
18,117
7<V93
21,171
5>'45
14,172
2,750
14,718
1,076,711
1,095,401
1,096,719
757,227
9 II ,37'
701,423
914,074
938,331
926,049
1,138,128
5 2 5>37 2
611,518
169,396
231,540
212,001
183,621
190,067
129,258
33 1, 909
46,301
160,357
155,046
104,236
127,535
106,893
109,522
134,110
1 7 2 ,755
121,320
1 82,002
23,562
7 6 ,384
48,014
47,402
83,771
40,089
19,779
28,391
11,204
78,122
1,801,325
1,962,426
M3 6 ,482
1,253,897
1,335,207
1,037,800
1,272,202
1,271,485
1,405,200
1,404,553
IQII
I.I2Q.C78
C8.4CQ
I 7 7.4 CO
42,246
1,363,733
IQI2
I.4.IO.84.O
84,181
I4O,I22
27,797
1,695,140
IQII
I,268,OC4
60,252
177,74!
29,271
1,534,918
IQI4
1^88,718
47.77 C
I74.IC2
25,408
1,596,073
IQI C
1 .24.0.804.
74.827
86,564
7O.I C2
1,392,343
ioi6
i,c86.qoo
88,802
124,700
50,259
1,850,661
IQI7
i ,704,706
Cq,6ll
170,610
515,113
2,109,139
1918
A(\\ C7I
6c occ
80 Q2C
110.646
IQIQ
I 2O CIQ
u iy;) j
247. C87
84.2 Q42
247,278
i y i y
IQ2O
06 QA.1
I.lo6.l6Q
2,HQ.6o2
902,108
iy*\j
IQ2I
y^yy^o
264,000
IO22
268,000
ly-Ax
IQ27
303,000
A y x j
IQ24
238,000
iv/xq.
IQ2C
118,000
*y*3
1926
204,000
IO27
74,000
*y*/
1928
216,000
IO2Q
787,000
iy-ty
TQOQ
13,000
i yj w
TOOT
31,000
i yj 1
IQ72
14,000
x yj-*
THE LIQUOR INDUSTRY
339
i>
c^ co ON >^ ON **"> O ON *^>oo
i:
c< M vo vo ^o vo co ^ * * O oo * *
>^Oco coO co t^.co'*cON''
c
Q
c* Os ON co Tfvo c< O O t^-VO oo cooo c* vo < ^-
cu
-Q
3
00 Tf HH O 00 c< vr COVO ^nc<Oc<vr,i-irt->-i ' '
HicOTt-ooooOQvOf^c<vooovo>-iOvooo * '
^Hcot^^^r^o^o t~^vo ^vo co co ^ d *-o *
::::::::::
U
MMH.M H,VO^- ;;
co
^MCOCOCO^^-CSCS "fONON COVO r- ^- co
r^
>
"g.S
O O c< ON^t <1 ^>ONONO t * ONOO HH ON -ooo r^ CO *
V5
D
Is
^-^OvO-> ^-w^Oc^vo Tl-cl^^vO O ^ON '
oo
^ .........
O
c^|
oo
i i
cT
00 + ~ r-- ^-00 unvo ON^HH ONOO OM^OM^
00
0?
TD
VO *-^*t^-OO O ^C^VOVO >- '^'^^O ^'CA CA VOQ
ctf
o
C
'.'.'.'.'.'.'.'.'.
h
?
&
rt
oo *-*" oo O O d co *-o ^J* O t^-vo oo vo oo d ON
t
"a
co i -oOcoONClOvo v/ ~>ctt^co-tt- ONOco '
2
v? ^vo "o ct^ \o" C^oo cTSooS^- ^-^co'
&H 'w'
m
*~COC*<S<S~C<C<~COVO gs ;
J *
s =a
VO *^
a M
s
^ . . . ^
*B
S
00 ' '
B.s
PQ
SS
2 w
C -rj
^vo O ^n t^ . vo . . ONOO
3 g
Q tJ
rt S
"5
M rt
Q CO
PQ *""*
? :
^ b
O oo co
Srt
M
8P
t"** co co
U
^
>
^s >ic
3
OS
* . . oo co^ON + . .
'&
co ' ' ON O\ ON t^ oo ' *
>
' co O i-t 00 VO * '
%
\
<3
3
vo ONOO ....ON vo ~oo O ~l^coco.
W
^
C!j
'5?
coco>- r^ ci ri-Moodvo r-oo *
PQ
^
H ^t ^ M r- -^ covo *
/<
O oo co
H
3
.00 O co^fH,.
'CO CO OO*o'*
<
r*>co<s''
^
^^ r^co 0,0 ~ *, r^cc cso -
co rf vnxo 1^00 ON O
V
ON0^0^8^0^0^0^0^0NO^O^O^ONONO^ONO^O^O^
O\ONO\O\ONO>ONONONON
340 STATISTICS OF THE LIQUOR INDUSTRY
o Q-VO *< r-vo
co Osvo Q r-- "
-
HI HI VOVO ^-00 vort-OO CO ">* O
r- ro O^oo vooo vo "* oo t^vo co
O
6\
o
cT oo" o^
<s vo
v
cf cT cT i-T >-T n i- c w i-
''U
vo vo
-i ^
VO VO
'
i ON OS OS ON OS O\
THE LIQUOR INDUSTRY 341
h * M H< vn c* O ONOOO covo oovnt^r-.co-ico>-irhOsc< O
^i^Mxy^wi^wQcoONr^ocJi-tt-ico^^eipdci^ p
__ M M M CO C** ^^^^^^^gjE
-( v^ ONOO
^> co cT co O
d
c^
^ tr\ w> r-} cf . O
1
I
R
53
!t ( CO
W
J
5 - P ......
^ |g S;:?o5.MS ?>?)s5."i?ta:u .q>^
5
8
o~
I_
cooo w^vndoo cooovo O rj-mcooo ONQ^
vo M co *n r^ O ^3 *^ M oo_ co ^n *-ovo
M HI M
g
^
342 STATISTICS OF THE LIQUOR INDUSTRY
TABLE 35. IMPORTS OF DISTILLED SPIRITS AS SHOWN BY THE REPORTS OF THE
BUREAU OF FOREIGN AND DOMESTIC COMMERCE, FISCAL YEARS 1901 TO 1932, INCLUSIVE
Year
Returned
Brandy
Whiskey
Gin
Cordials
and
liqueurs
All other
Total
IQOI
Gallons
87C.OQQ
Gallons
2QO.'JOI
Gallons
Gallons
Gallons
Gallons
I.7I2.I<6
Gallons
2 877. CC6
AVfVA
IQO2
w / j> w yy
8OC.2I2
716,222
1.000,887
7.O7I 721
IQOI
810 CQI
04.8.878
2 o6l OC7
7 22Q C26
*y^O
IQO4
"*y>j;X*
4.7I.CQ6
^00,088
2.278.842
3IOI A26
IQOC
116.4.60
AO'i,'i86
2.766^4.66
7.O86.72I
1006
I77.4.QQ
4.70^1^7
2,670.680
7.287.612
IQO7
i <4..io6
620,777
7.27O.226
4..o<7 66 c
*y w /
1008
148,208
CQ2.784
7,2l6.228
7.QC6 QIO
IQOQ
TOJ. OI C
^^A-lAA
7.88Q.O66
4. 787 72C
*yy
IQIO
*J'T> W<1 J
1 1 Q. 6/l6
7 1 6.2 CO
1.060.700
1,240.662
I.24C.2OO
T->/ />j *:>
4 782 o67
Ay*v*r
IQII
4.00,24.2
1,207,602
I,O4C,8l<
Q2C,6oi
7.674. 7 CO
IQI2
<OQ,286
i,777,oio
824,694
C72.ICI
4II,CQC
7.6CO.776
IQI7
6io,7c8
1,541,663
074,776
c7<r,2Qo
778,627
4,080,710
IQI4
602, <6 7
1,01,870
i.occ,88c
<K,<7<
4l4,qCO
4,160.847
IQIC
4OO.2O7
I,727,7Cq
742,470
408, OQO
411,276
7,28q.727
1016
C76,742
1,742,197
8OC.74Q
77O.4C2
C78,7CQ
7. oc 7.4.00
IQI7
420, ^67
1,676,151
267, C2O
7C7.7II
397,934
7,IIC,487
iqi8
274,QI2
706.267
112,649
76,I2O
154,148
I,774,Oq6
IQIO
224
2,964
7,188
IQ2O
28.QIQ
167.710
27,287
<8,4Q7
4,66 c
282 674
IQ2I
487
*y-**
IO22
64
jy^^r
IQ27
CO
*y*J
IQ24
<7
IO2C
<8
*7 J
IQ26
72
*y-* w
IQ27
70
*y*/
1028
7Q
*yxu
I02Q
8l
IQIO
47
*yj v
TOOT
77
*yj*
IO12
70
THE LIQUOR INDUSTRY
343
TABLE 36. APPARBKT U. S. CONSUMPTIOX or DISTILLED SPIRITS, 1901 TO 1932
[Statement in tax gallons]
Year
Withdrawals
Imports
Exports
Apparent
consumption
1901
60,585,730
2,877>556
1,801,325
61,661,961
1902
58,611,443
3,3 I *32i
1,962,426
59*680,338
1903
49* 1 56*305
3,229,526
1,536,482
50,849,349
1904
49,762,264
3,101,426
1,253,897
5^609,793
1905
49*59M83
3,086,321
1,335*207
51,342,697
1906
54,316,160
3,287,612
1,039,800
56,563,972
1907
64,390,492
4,053,665
1,272,202
67,171,955
1908
60,996,474
3,956,910
1,271,485
63,681,899
1909
67*250*3*7
4,787>3 2 5
1,405,200
70,632,442
1910
72,994,478
4,382,067
i *Q4,553
75*971,982
1911
78,894,261
3*674,350
1,363,733
81,204,878
1912
78,949>488
3*650,736
1,695,140
80,905,084
1 9 1 3
83,577*326
4,080,710
i,534,9 l8
86,123,118
1914
80,065,262
4,160,843
1,596,073
82,630,032
1915
70,152,366
3*289,727
1,392,343
72,049*750
1916
77>076,536
3,953,499
1,850,661
79* J 79*374
1917
93*210,559
3," 5>483
2,109,139
94,216,903
IQl8
60 .76 1. 2 "7O
I.174..OQ6
62. 1 7C.726
y w
iqlq
w,y v * j.^jv
65,625,796
*,O/^ -7
3,188
v , O J,J
65,628,984
y y
IQ2O
6.7Q4..807
282,674.
6.677x71
-?
1921
^joy^* v y /
9,258,500
, /^
487
264,000
> / /, J /
8,994,987
1922
2,718,534
64
286,000
2,432,598
1923
13,007*432 *
50
303,000
12,704,482
I92 4
19,813,322 *
53
238,000
19*575*375
1925
35* 1 56,785 *
58
118,000
35*038,843
1926
52,586,654 *
72
294,000
52,292,726
1927
43*876,34* *
70
34,000
43,842,412
1928
40,191,134 *
79
216,000
39*975.213
I92 9
52,o33,!7o *
81
383,000
51,650,251
1930
47,402,120 *
43
13,000
47>3 8 9* l6 3
1931
34,281,295*
33
31,000
34,250,328
I 93 2
24,476,341 *
39
14,000
24,462,380
* Includes 25% of alcohol production estimated as used by bootleggers.
344 STATISTICS OF THE LIQUOR INDUSTRY
O
W
P
Q &
55 >->
13
O
B 2
S 5
o
Q
<
I) e
g
1
s J,
1.9
s >
3? 2
JJ g
> 3^
6c
iq
c
.2
O
to
ON O
Osvo Q vo O o c< M ONVO
^-t^ONOOnvncovo^oONCXJ
o oo <> o \o r^- 4- o 4-
r^ONCOOO>
-
M o oo
Q M
O Os
-< -ncoH
oooooooooo
<-o vo O O O^-^O O *^>vo
vo M ro co cs c so o\ oo t^.
c n c oc
rh
oo
^ S>^
ON ON ON ON ON ON ON ON ON ON C3N ON ON ON ON ON ON ON ON ON ON
ci
ON
THE LIQUOR INDUSTRY
345
TABLE 38. WINE EXPORTS AS SHOWN BY THE REPORTS OF THE BUREAU OF
FOREIGN AND DOMESTIC COMMERCE, FISCAL YEARS 1901 TO 1925, INCLUSIVE
Year
Gallons
Year
Gallons
Year
Gallons
Year
Gallons
1901
1,147,561
1908
457>495
1914
941,357
1920
4,573,587
1902
962,756
1909
427,408
1915
819,310
1921
26,000
1903
693,846
1910
5i9, 2 34
1916
1,133,274
1922
12,000
1904
914,841
1911
J , 394,994
1917
2,245,013
1923
47,000
1905
856,786
1912
957,120
1918
2,765,344
1924
13,000
1906
806,314
'9*3
1 WS 1 S 1
1919
4,926,425
1925
14,000
1907
573,359
346 STATISTICS OF THE LIQUOR INDUSTRY
TABLE 39, WINE IMPORTS AS SHOWN BY THE REPORTS OF THE BUREAU OF FOREIGN
AND DOMESTIC COMMERCE, FISCAL YEARS 1901 TO 1931, INCLUSIVE
Year
Still wines
Champagnes
and other
sparkling
wines
Total
Gallons
Gallons
Gallons
1901
3,9 7,346
933,234
1902
4,493,48o
995,768
1903
5,075,818
,223,832
1904
5,421,150
,008,735
1905
5,440,238
,"5,433
1906
6,122,563
,246,182
1907
7,124,272
,258,209
1908
7,329,066
,100,007
1909
7,699,639
1,309,884
1910
9,567,390
1,173,009
1911
6,602,350
665,485
1912
5,595,802
843,402
1913
6,461,5^3
842,484
1914
7,405,289
810,006
1915
5,740,868
343,890
1916
5,094,113
618,630
1917
4,770,606
587,142
1918
3,604,335
372,690
1919
251,865
27,822
1920
723,723
96,861
1921
1,446,809
122,942
i,569,75i
1922
645,987
32,652
678,639
1923
161,510
J 3,959
175,469
1924
90,721
2,209
92,930
1925
79>7i3
1,926
81,639
1926
63,033
13,946
76,979
1927
33,337
3,545
36,882
1928
33>497
1,911
35,408
1929
34,2ii
1,298
35,509
1930
28,196
1,238
29,434
I93 1
26,306
!,343
27,649
THE LIQUOR INDUSTRY
347
TABLE 40. APPARENT CONSUMPTION OF WINE IN THE UNITED STATES, FISCAL YEARS
1912 TO 1932, INCLUSIVE
Year
Gallons
Year
Gallons
1912
57,059,000
1923
14,812,000
*9 1 3
55,988,000
1924
9,112,000
1914
53,189,000
1925
3,701,000
1915
33,341,000
1926
5,890,000
1916
47,942,000
1927
4,434,000
1917
42,999,000
1928
4,974,000
1918
52,242,000
1929
11,416,000
1919
51,110,000
1930
3,200,000
1920
16,329,000
I 93 l
6,680,000
1921
21,989,000
1932
5,243,000
1922
6,538,000
TABLE 41. INTERNATIONAL TRADE IN WINES 1930
(In thousands of gallons)
Country
Production
Imports
Exports
France
I.IOQ.Q77
7C2,78i
28.014
Italy
i*777
404
27.267
Spain
JJ *)/O/
48i,c8c
'ry'r
VI
*/>* w j
02.200
Algeria
7CQ,7I4
838
2Q7.1 7 C
Roumania
22I.C42
IO
7A
Argentina
165,000*
1,512
JT
144
Portugal
lCC,66q
17
21,607
Hungary
*jjy j 7
oc.626
27
8,26 c
Germany
66.QOC
21,074
I.7Q4
Bulgaria
62.417
f
2
Austria.
71,768
0,8 co
17
Australia
1 8.1 co*
c8
470
Switzerland
l6QOQ
70,002
60
* Estimated.
f Less than 1,000 gallons.
Source: International Yearbook of Agricultural Statistics.
SELECTED BIBLIOGRAPHIES *
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Technischer Vortraege. Vol. II. Stuttgart, 1902.
ALLEN, PAUL W. Industrial Fermentation. New York, 1926.
BITTING, K. G. Yeasts and Their Properties. (Purdue Uni-
versity Monograph Series, No. 5.)
BUCHNER, E. H., and M. HAHN. Die Zymase Gahrung.
Miinchen, 1903.
EFFRONT. Biochemical Catalysts. New York, 1917.
GREEN-WINDISCH. Die Enzyme. Berlin, 1901.
GUILLIERMOND, A. The Yeasts. New York, 1920.
HANSEN, E. CHR. Practical Studies in Fermentation. London,
1896.
HARDEN, ARTHUR. Alcoholic Fermentation. London, 1923.
HENRICI, A. T. Molds, Yeasts, and Actinomycetes. New
York, 1930.
JORGENSEN. Micro-Organisms of Fermentation. London, 1900.
KLOECHER. Fermentation Organisms. London, New York,
1903.
LAFAR. Technical Mycology. London, 1910.
MAERCKER. Handbuch der Spiritusfabrikation. Berlin, 1908.
MATTHEWS, CHAS. G. Manual of Alcoholic Fermentation.
London, 1901.
OPPENHEIMER. Dis Fermente. Leipzig, 1913-29.
RIDEAL, SAMUEL. The Carbohydrates and Alcohol. London,
1920.
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included here, except whiskey, in: West and Berolzheimer. Bibliography of Bibli-
ographies on Chemistry and Chemical Technology. Washington, 1925, 1929, 1932.
348
SELECTED BIBLIOGRAPHIES 349
DISTILLATION. PRACTICAL AND THEORETICAL
ELLIOT, C. Distillation in Practice. London, 1925.
ELLIOT, C. Distillation Principles. London, 1925.
HAUSBRAND, E. Principles and Practice of Industrial Distilla-
tion. Trans, from the 4th German ed. by E. H. Tripp.
London, 1925.
ROBINSON, C. S. The Elements of Fractional Distillation. New
York, 1930.
YOUNG, SYDNEY. Distillation Principles and Processes. Lon-
don, 1922.
ALCOHOL
FARMER, R. C. Industrial and Power Alcohol. London, 1921.
FOTH, GEORGE. Handbuch der Spiritus Fabrikation. Berlin,
1929.
FRITSCH, J., and VASSEUX, A. Traite Theoretique et Practique
de la fabrication de L'alcool et de Produits Accessoires.
Paris, 1927.
MclNTOSH, JoHN^G. Industrial Alcohol. London, 1922.
SIMMONDS, CHAS. Alcohol: Its Production, Properties, Chem-
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DE VOL, EVERETT T. A Farmers' Practical Treatise on Fer-
mentation, Distillation and General Manufacture of Alcohol
from Farm Products with Subsequent Denaturing. Omaha,
1921.
WRIGHT, FREDERICK B. Alcohol from Farm Products. New
York, 1933.
DISTILLED LIQUORS
DE BREVANS, J. La Fabrication des Liqueurs. Paris, 1897.
FOTH, GEORGE. Handbuch der Spiritus Fabrikation. Berlin, 1929.
KULLMANN, OTTO. Die Spirituosen Industrie. Leipzig, 1912.
MACDONALD, AENEAS. Whiskey. Porpoise Press, Edinburgh,
1930.
PIAZ, A. DAL. Die Cognac und Wein Spirit Fabrikation so wie
die Trester und Hefebranntweinbrennerei. Wien, 1891.
ROCQUES, X. Les Eaux-de-vie et Liqueurs. Paris, 1898.
350 SELECTED BIBLIOGRAPHIES
ROGERS^ ALLEN. Industrial Chemistry. New York, 1926.
SCHEDEL, C. F. B. Der Distillateur. Leipzig, 1921.
WINES
ALWOOD, WILLIAM B. Experiments in cider making applicable
to farm conditions and notes on the use of pure yeast in
wine making. Bull. 129, U. S. Bur. of Chem., 1909.
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Kellerwirtschaft, 4. Auflage. Berlin, 1910.
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Stuttgart, 1903,.
BENEVEGNIN, LUCIEN, and others. Manuel de Vinification.
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BIOLETTI, FREDERICK T. Defecation of Must for White Wine.
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Countries. California Agricultural Experiment Station,
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BIOLETTI, F. T., and CRUESS, W. V. The Practical Application
of Improved Methods of Fermentation in California Wines
during 1913 and 1914. California Agricultural Experi-
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BIOLETTI, F. T. The principles of wine making. California
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methods of fermentation in California wineries during 1913
and 1914. California Agricultural Experiment Station,
Circ. 140. 1915.
BOULLANGER, EUGENE. Distillerie Agricole et Industrielle
Eaux-de-vie de Fruits. Paris, 1924.
DE BREVANS, J. La Fabrication des Liqueurs. Paris, 1897.
SELECTED BIBLIOGRAPHIES 351
COSTE-FLORET, P. Precedes Modernes de Vinification.
1. Vin Rouges. Paris, 1899.
2. Vin Blanc. Paris, 1903.
3. Les Residus de la Vendage. Paris, 1901.
CUNIASSE, L. Memorial du Distillateur Liquoriste. Paris,
1925-
DUBOR, GEORGES DE. Viticulture et Vinification Moderne.
Paris, 1894.
EMERSON, E. R. The Story of the Vine. New York and Lon-
don, 1902.
FRITSCH, J. Nouveau Traite de la Fabrication des Liqueurs.
Paris, 1926.
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HAYNE, ARTHUR PERONNEAU. Bull. 117, Agricultural Experi-
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HUSMANN, GEORGE, and others. American Grape Growing and
Wine Making. New York, 1919.
KULISCH, P. Sachgemasse Weinverbesserung. Berlin, 1903.
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Schaumwein. Leipzig, 1913.
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SCHMITTHENNER, F. Weinbau und Weinbereitung. Leipzig,
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352 SELECTED BIBLIOGRAPHIES
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VISETELLY, HENRY. A History of Champagne with Notes on
other Sparkling Wines of France. New York and London,
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WILEY, HARVEY W. American Wines at the Paris Exhibition
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Weinbereitung und Kellerwirtschaft. Berlin, 1905.
ANALYSIS
CUNIASSE, L. Memorial du Distallateur Liquorist Paris,
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LEACH, A. E. Food Inspection and Analysis. New York, 1920.
PRESCOTT, ALBERT B. Chemical Examination of Alcoholic
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SELECTED BIBLIOGRAPHIES 353
ROSENHEIM, OTTO, and SCHIDROWITZ, PHILLIP. On some
Analyses of Modern "Dry" Champagne. In the Analyst
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for the Determination of Esters, Aldehydes and Furfural
in Whiskey. Jour. Am. Chem. Soc. 28, 1619-29 ( 1906).
WILEY, H. W. Beverages and their Adulteration. Philadel-
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STATISTICS
Bureau of Industrial Alcohol. Statistics Concerning Intoxica-
ting Liquors. U. S. Treas. Dept. Washington, 1932.
International Yearbook of Agricultural Statistics. Rome, 1930.
ROLLER, ARNOLD. La Production et la Consommation des
Boissons Alcooliques dans les Different Pays. Bur. Internat.
Centre L'Alcoolisme. Lausanne, 1925.
Rep. of the Bur. of Foreign and Domestic Commerce. U. S.
Dept. Comm. Washington, 1901 date.
INDEX
Absinthe, 203
Acetaldehyde, 22, 23
Acid-alcohol ratio in wine, 259
Acid conversion process, no, in
Acidity, charge during fermentation, 168
function of, 162
total, determination of, 278, 288
volatile, determination of, 279
Aging, artificial, 128
British practice, 128
charred barrels in, 128
of liqueurs, 194
President Taft*s report on, 128
Snell & Fain on, 129
Agrafe, 183
Agricultural products, consumption of,
330, 334, 335
Alcohol, boiling curve of, 80
crude, neutralization of, 90
determination of, 261, 287
distillation curve of, 81
Alcohol-extract ratio in wine, 259
Alcohol, immersion refractometer tables,
308-319
in cider, 188
recovery of, 127
specific gravity tables, 302-307
steam used for, 95
theoretical yield, 18
yield from barley, 29
yield from corn, 32
yield from oats, 33
yield from rye, 30
"A I cool d'industrie" 140
Aldehydes, 91
determination of, 288
Alembic des lies, 142
Alkalinity of ash, 276
Alkermes de Florence, 204
Amines, in alcohol, 91
Amino-acids, role in fermentation, 23
Amyl alcohol, 23, 24
Amylase, 10
Amylopectin, 1 1
Amylose, 1 1
Anaerobes, 58
Analysis, reasons for, 230
"Analyzer," 87, 90
Angelica liqueur, 204
Angostura Bitters, 226
Anisette, 205
Applejack, 152
Apple, varieties, 188
"<i premier-jet" still, 141
Arrack, 153
Ascospores, 48
Ash, alkalinity of, 276
determination of, 275, 287
Ash-extract ratio in wine, 275
Aspergillus Niger, 56, 57, 58
Autolysis, 14, 19
Bacteria, disease, 55, 59
effect of SO2 on, 62
Barley, average composition of, 28
botanical description, 28
Barley grain, cross-section of, 72
yield from, 29
Bath-tub gin, 150
Bead, 128
Beer still, 90, 91
operation of, 92
"Benedictine," 208
Bitters, 226
Black currant brandy, 209
Black mold, 57, 58
Blended whiskey, definition, 233
Blending of liqueurs, 192, 193
of whiskey, 136
Blue mold, 56
"bonne chauffe/' 141
Botrytis cinerea, 56, 57, 58, 59
Bourbon whiskey, aging of, 129
description, 99
Brandies, analyses of, 292, 293, 294
Brandy, aging of, 142
blending of, 142
classification of, 140
description of, 139
distillation of, 141
dosing of, 143
F.A.C.A. definition, 235
wine for, 142
British brandy, 143
"Bronillis/' 141
Brou de Noix, 219
Burnt ale, 105
Cane sugar solutions, density of, 298-301
"Cap" on fermenting wine, 168
Caramel, detection of, 295
Caramel malt, 74
356
INDEX
Carbohydrates, 4
Carbon dioxide in champagne, 181
Carboxylase, 22
Cassis, 209
Catalysis, 13, 14
Cent Sept Ans, 220
Cereal grains, average composition, 36
"Cerelose," 10
Champagne, dosage of, 179
manufacture of, 180
pressure of, 183
Changes during fermentation, 168
Chaptalizing, 176
"Chartreuse," 210
"Chauffe <vin } " 83, 141
Cherry cordial, 212
Chlorides, determination of, 277
Chlorophyll, 46
Cider, 187
Clarification of liqueurs, 196
Cocoa, cream of, 213
Co-enzymes, 15, 16
Coffee, cream j>f, 213
"Coffey" still, 87
Cognac, F.A.C.A. definition, 235
Color of grapes in wine, 168
Color, insoluble in amyl alcohol, 295
water insoluble in whiskey, 293
Coloring of liqueurs, 196
Coloring, permitted, 241
Colors, vegetable, synthetic, certified,
44
Column still, 87 . .
Compound gin, F.A.C.A. definition, 235
Concentrating column, 94
Conge, 192
"Conge in trancher" 194, *95
Consumption of distilled spirits, 328, 343
Consumption of wine, 329
Cordials, 190
analyses of, 259
methods of analysis suggested, 297
U. S. Dept. Agr. definition, 229
Corn, average composition, 32
description, 31
varieties, 31 .
Corrections of wine, permitted, 238
"Corty's head/' 86, 87
Cream of absinthe, 203
of Vanilla, 225
Creme d' Ananas, 222
Creme de cacao, 213
Creme de celeri, 210
Creme de Fleurs d'Oranger, 220
de Menthe, 218
de Moka, 213
Creme de Noyaux, 220
Crushing of grapes, 166
Curasao, 214
manufacture of, 200
Cuvee, 181
Cytase, 72
Defecation of grape must, 67
Dematium pullulans, 54, 56, 58
Demerara rum, 147
Density of sugar solutions, 298-301
Dephlegmator, 92
Dessert liqueur, 216
Dextrin, 10
Dextrose, 5
Diastase, 10
Diastatic power, 74
Diatomaceous earth, 189
Dihydroxy-acetone, 21
Disaccharides, 4
Distillation, alcohol recovery in, 95
definition, 79
Distillation of liqueurs, 192
Distillation, steam used for, 95
Distilled, gin, F.A.C.A. definition, 234
Distilled spirits, production of, 327,
336
Distiller, illicit, 97
Distilleries, registered, member of, 331
Dop brandy, 140
Dry wine, definition, 158
U. S. Dept. Agr. definition, 236
Dunder, 146
"Eau de vie" 140
de Dantzick, 217
de Hendaye, 217
"Eau de vie de marc" 140
Egg white, in fining, 178
Elixir de Garus, 216
Embryo, 71
Endo-sperm, 71
Enolic acids, 168
Enzymes, classification, 14
description, 13
preparation, 15
specific, 13
Essence, 43
Essential oils, defined, 43
origin, 43
Esters, determination of, 288
Exhausting column, 93
"Export trade" rum, 144
Exports, of distilled spirits, 338, 339-
34i
of wine, 345
Extract, determination of, 266, 287
Feints, 90, 105, 107^
Fermentation, aeration in, 105
completion of first, 169
general requirements, 17
Lavoisier's formulation, 18
open or submerged, 168
INDEX
357
Fermentation, Pasteur's formulation, 18
products of, 1 8, 19
rate of, 19
temperature variation of, 19
Filtration of liqueurs, 198
Fining of liqueurs, 196
Fining of wine, 176
Flavoring Agents, classified, 41
Flavoring, permitted, 241
Foreign trade in distilled spirits,
327
Foreshots, 105, 107
Fortified wine, definition, 158
U. S. Dept. Agr. definitions, 236
Fractional distillation, 79
French Vermouth, 228
^-Fructose, 5
Fungi, 46
Furfural, determination of, 289
Fusel Oil, 18, 23, 90
determination of, 290
Galactose, 5
Gallizing, 176
Garus' Elixir, 216
Gas pressure, in champagne, 183
Gelatin, in fining, 178
in fining liqueurs, 198
Geneva gin, 149
Gin, analysis of, 256
F.A.C.A. definition, 234
"Gin head," 149
Gin still, 151
^/-Glucose, 10
Glucose, commercial, 10
Glyceraldehyde, 21
Glycerol, 18, 22
Glycerol-Alcohol Ratio, 266
Glycerol in wines, determination of,
262-266
Glycogen, 21
Golden Elixir, 217
Grand mousseaux, 183
Grape juice, changes during fermenta-
tion, 164
Grape pomace, brandy from, 140
Grapes, American Varieties, 38
crushing of, 166
for champagne, 180
not recommended, 40
planted in U. S., 37
recommended, 40
stemming of, 165
yield per acre, 39
"Grappo," 140
Gray mold, 57
Green chartreuse, 210
Green malt, 77
Guianolet d* Angers, 213
Hamburg brandy, 143
Hemicellulose, 12
Hendaye's Elixir, 217
Hexabioses, 6
Hexose, 4
Hexose-di-phosphate, 20
Holland Gin, 149
"Home trade" rum, 144
Hot feints, 90
Huile de Kirsc/twasser, 218
Huile de roses, 223
Imitation champagne, 187
Imitation liquors, F.A.C.A. definitions,
240
Immersion refractometer tables for al-
cohol, 308-319
Immersion refractometer table for wood
alcohol, 294
Imports, of distilled spirits, 342
of wine, 346
Infusion, description, 192
Infusions, grades of, 209
International trade in wine, 347
Invertase, 16
Irish whiskey, 100
F.A.C.A. definition, 234
manufacture of, 103
Isinglass, in fining liqueurs, 197
in fining wine, 177
Italian Vermouth, 228
Jamaica rum, analyses of, 254, 255
manufacture of, 144, 145
Kirschwasser Liqueur, 217
Kornbranntwein, 154
Lactacidase, 21
Lactic acid, 21, 22
Lactic acid bacteria, 59
use, 65
Lactose, 5, 6
Laevulose, 5
Lipase, 16
Liqueur de Dessert, 216
Liqueurs, analyses of, 259
classification, 190
methods of analysis suggested, 297
operation in manufacture of, 192
Liqueurs par distillation, 191
par infusion t 191
"Local trade" rum, 144
Low wines, 84, 105, 107
"Lyne arm," 107
Maize, 31
Malt, definition, 71
drying, 77
358
INDEX
Malt, green, 77
steeping for, 75
Maltase, 10, 16
Malting, changes during, 73
compartment system, 77
drum system, 76
end of, 74
floor system, 76
yield in, 78
Maltose, 5, 10
Mash tun, 102
Mashing, 101, 104
American practice, 117
Mass Action Law, 17
Massecuite, 146
Methanol, detection of, 296
Methyl alcohol, determination of, 291-
293
Methyl-glyoxal, 22
Milk, in fining liqueurs, 198
in fining wine, 177
Molasses, 146
Molds, 52, 56
Monosaccharides, 4
Mucor, 56
Munson and Walker's Table, 320-325
Must, 51
sterilization of grape, 173
wine, composition of, 162
Mycoderma vini, 54, 55, 58
Neutral whiskey, definition, 233
"Nigger rum," 144
Nitrates, in wine, detection of, 286
Nitrogen, determination of, 282
"Noble Mold," 57
Noyaux, 219
Oats, average composition of, 33
occurrence, 32
yield from, 33
Open fermentation, 168
Orange flower cream, 220
Oxydase, 57
control of by SO2, 62
Oxygen, 17
Parfait Amour, 221
Patent still, 87, 88
yield from, 114
Pelargonic ether, 148
Penillium glaucum, 56, 58, 59
Pentosans, determination of, 2^3-285
Pepsin, 13
Phosphates, role in fermentation, 20
Phosphoric acid, determination of, 277
Pineapple Liqueur, 222
Pinette, 170
Plaster of Paris, in wine, 175
Plumule, of malt, 74
Polysaccharides, 4
Pot ale, 105
Potassium metabisulphite, use of, 174
Pot still, with rectifier, 85
yield from, 113
Production of distilled spirits, 327, 336
Protein, determination of, 282
role in fermentation, 24
Proteolysis, 72
Protoplasm, 46, 47
Pseudo-yeasts, 52, 54
Punch Liqueur, 222
Pyruvic acid, 22
Quince Brandy, 222
Racking, 171
Raffinose, 4, 15
Ratafia de cassis, 209
Ratafia de cerises, 212
de Goings, 222
de FrambroiseSj 223
Raw Materials, classification, 25
Rectification, definition, 79
Rectifier, 90
Recuperator, 92, 94
Red wine, difference from white wine,
159
manufacture of, 163
Reflux, definition, 79
Refractometer, immersion, table for
wood alcohol, 294
tables for alcohol, immersion, 308-319
Resins, in alcohol, 91
Rose liqueur, 223
Rum, analyses of, 254, 255, 256
classification of, 144
description of, 143
essence, 148
Rye, average composition of, 30
botanical description, 30
yield from, 30
Rye whiskey, aging of, 129
description, 99
Saccharomyces apiculatus, 53, 54, 55, 58
cerevisiae, 50
ellipsoideus, 49, 51, 53, 54
mycoderma, 51
pastorianus, 51, 53, 54
Saccharose, 5
Schnapps, 154
Scotch whiskey, 99
F.A.C.A. definition, 233
manufacture of, 103
Secondary products, in whiskey, 109
Seeds, average composition, 36
Simple distillation, 79
"Smoothen," 149
Sour mash, 100
INDEX
359
Sparger pipe, 93
Sparkling wine, definition, 159
U. S. Dept. Agr. definitions, 237
Specific gravity, determination of, 260,
286
tables for alcohol, 302-307
Spent lees, 105
Spirit plate, 90
Spirits, in bond, 333
Spores, 48
Starch, acid conversion, 78
classification of granules, 7
conversion, 9
hydrolysis, 9
pressure cooking of, 117
properties, 7, 8
thick or thin-boiling, 8
Starters for wine, natural, 67
preparation, 67, 68
pure culture, 68
Stemming, 165
Still, continuous rectifying, 93, 94
definition, 79
simple pot, 82
unique, 97
Still wine, definition, 159
Straight whiskey, F.A.C.A. definition,
233
Strawberry cordial, 223
Submerged fermentation, 168
Sucrose, 5
determination of, 271
Sugar cane juice, composition of, 145
Sugar, density of solutions, 298-301
function of, in must, 162
Sugars, determination of, 267-275, 291
Sulphuric acid, determination of, 277
Sulphur, use of, 174
Sweet mash, TOO
Sweet wine, definition, 158
U. S. Dept. Agr. definition, 236
Tannin, addition of, 176
determination of, 281
function of, 162
Tartaric acid, 168
determination of, 280
Taxes, collected on liquor, 332, 344
Tirage, 183
Torulae, 54
"Tranchage" 194
Trappistine, 223
Trisaccharides, 4
Turpentine, in gin, 150
Unfortified wine, definition, 158
Unicurs Bitters, 27
Urease, 13
"Usquebaugh," 96
Vacuoles, 47
Vat stills, 147
Vermouth, French, 228
Italian, 228
Vespetro, 224
Vinegar bacteria, 59
Vodka, 154
Volatile acids, determination of, 279
Wash, 84
Wash stills, capacity of, 85, 107
Water, use of, 103
Wheat, average composition, 35
botanical description, 34
classification, 34
Whiskey, analyses of, 242-251
blending of, 136
Bourbon, description, 99
conclusions from analysis of, 249,
252
definition, 99
distillation of, 105, 106
dosing of, 134
F.A.C.A. classification, 232
F.A.C.A. definitions, 233
fermentation of, 104
Irish, loo
origin, 96
patent still, British, 107
recovery of, 112
rye, description, 99
Scotch, 99
sour mash, 100
statistics on, 333-341
sweet mash, 100
tax history, 96, 97, 98
U. S. Pharmacopoeia requirements for,
232
yield of, 112
Whiskey types, 102
White chartreuse, 211
White wine, difference from red wine,
159
manufacture of, 173
Wine, acid-alcohol ratio in, 259
aeration of fermented, 172
alcohol-extract ratio in, 259
classification of, 158
conclusions from analysis of, 256,
259
consumption of, 329, 347
correction of, 175
defecation, 67
examination of, 260
extract in, 266
fining of, 176
functions of, 160
general definition, 155
industry, started in U. S., 37
360
INDEX
Wine, lees, 141
names considered, 157
pasteurization of, 172
plastering of, 175
pressing of, 170
starters for, natural, 67
starters for, pure culture, 68
statistics on, 344-347
U. S. Dept. Agr. definition, 235
Wines, analyses of, 257, 258
low, 84
Withdrawals, of distilled spirits, 337
Wort, American practice, 115, 117
for yeast production, 65
preparation of, 104
preparation for British whiskey, no
Yeast, commercial production, 63, 64
distiller's, production of, 65, 66
Yeast juice, 16
Yeasts, classification, 49
effect of alcohol on, 58
effect of SO2 on, 61
mode of growth, 47
pure culture, 50
relation to acids, 61
relation to oxygen, 60
relation to temperature, 61
wild, 50
Yellow chartreuse, 211
Zymase, 16
Zymogen, 15